Silk Road forums

Discussion => Off topic => Topic started by: Operation Shulgin on August 13, 2012, 04:36 pm

Title: Chemistry Discussion
Post by: Operation Shulgin on August 13, 2012, 04:36 pm
i'd love to see a chemistry section on SR, OVDB was a great read and everyone was quite serious. So what do you think?

Update: 14-8-2012

This thread was to see if there was interest in a chemistry section but thanks to YOU we have already have some great discussion, users submitting information and hopefully are going to continue to do so!

Here are some helpful links and documents:
Quote
Rhodium (The hive, Rhodium unfortunately the websites are down but erowid still has a archive of the website, great links anything from the plant --> sassafras --> Safrole -->  MDP2P to the actual product MDMA :)
http://www.erowid.org/archive/rhodium/chemistry/index.html

"Total Synthesis II" This is the scanned book which strike wrote, the document is in in PDF format, this is a must have with every step carefully explained (multiple methods for every step) a great read too!
(Run it sandboxed if you're paranoid)
https://thepiratebay.se/torrent/5188247/Total-Synthesis-II_(How_To_Make_Ecstacy)-by_Strike.pdf

"The Complete Idiot's Guide to Organic Chemistry" Don't let the name fool you! This book is fantastic just like TSII the author wrote everything in such a way that it's fun and addicting to learn!
https://thepiratebay.se/torrent/7001182/

"Sources by strike" I can't vouch for this book,i own it but i haven't read it yet! The book is about (and correct me if i'm wrong) how to obtain chemicals and such from sources
https://thepiratebay.se/torrent/5188269/Sources_-_by_Strike_%5B1998%5D.pdf

And last but not least (more to come..) Sandboxie, as you never know what these PDF's carry besides knowledge..
http://www.sandboxie.com/index.php?DownloadSandboxie
Title: Re: Chemistry Discussion
Post by: ZenAndTheArt on August 13, 2012, 04:49 pm
I loved the chemistry sections of Opiophile.org. The things those guy knew could be mind-blowing, not just about opiates either. I'd read a SR one, but I've nothing to contribute, sadly.
Title: Re: Chemistry Discussion
Post by: DiscountDank on August 13, 2012, 05:26 pm
Hey shulgin, I would love a chem section and I wish there were more precursor classifieds...I have a lot of info to contribute but also would like pointers and some advice on some reactions as well. 
Title: Re: Chemistry Discussion
Post by: Mashman on August 13, 2012, 06:18 pm
Yer I'd like to see a chem section too. Maybe a sticky somewhere?
Title: Re: Chemistry Discussion
Post by: le botbahn on August 13, 2012, 11:45 pm
Nomad bloodbath had to scold the meth review section earlier for the excessive "scholarly" chatter :P

Because it's meaningful discussion but derailing the thread, he mentioned cleaning the thread up & creating a new separate thread for all the Walter White chem talk. Maybe this would be a good place for some of that.
Title: Re: Chemistry Discussion
Post by: Mashman on August 14, 2012, 12:03 am
Well we might as well start it off then see what sort of interest we get?
Title: Re: Chemistry Discussion
Post by: dkmonk on August 14, 2012, 12:07 am
I would love, love, love a meth chemistry thread. There is a real good one on the shroomery that I would post in a lot and learned some things from people who were real chemists and knew a lot more than I ever could imagine which is what I like, because they can provide ways to improve what your trying to do and cut out unnecessary risks involved.

Title: Re: Chemistry Discussion
Post by: Mashman on August 14, 2012, 12:15 am
I would love, love, love a meth chemistry thread. There is a real good one on the shroomery that I would post in a lot and learned some things from people who were real chemists and knew a lot more than I ever could imagine which is what I like, because they can provide ways to improve what your trying to do and cut out unnecessary risks involved.

Well I'm from uk so don't really know much about meth. I saw something on tv about a method where it's all produced in a 2litre coke bottle. You know how that's done at all?
Title: Re: Chemistry Discussion
Post by: dkmonk on August 14, 2012, 12:20 am
Yah, I actually just posted how to do it that way in the meth vendor review thread, but it is irrelevant to the thread so I was scolded slightly.

There are many variations of the method, but this one is a collaboration of more than one person who actually understand the chemistry behind meth.
Title: Re: Chemistry Discussion
Post by: Mashman on August 14, 2012, 12:38 am
I've copied it from the meth thread DK if that's cool with you?

If you want to make it then I have a write up that I posted that was created by me and a few other people who were experienced with this kind of thing, so we could provide a more scientific and safe way to the birch reduction one pot method.

I made a thread with a write up on the one pot method that I thought was fairly decent, but there are a lot good tips that were posted in the thread from me and a few other people on the site where it was originally from that I wasn't able to paste, but really they aren't necessary and would just complicate things for a beginner such as the cold water batch, and using anhydrous sulphuric acid to smoke off with instead of just the regular out of the bottle stuff, so that you reduce H20 vapor contact, which is safer since H20 is the enemy in that process.

Here it is:

 "I liked this write up. Just ignore adding water. --- THIS IS IMPORTANT DON'T USE WATER IGNORE THAT PART

The Process:

After reading around about the lithium reduction and stumbling across the shake and bake method, I came up with this safe compromise.  Safety is paramount, that is number one.  I am well aware of the dangers of the RedPhos/HI method, a lot of cooking/filtering/condensing typically took me around 48 hours to do a batch from start to finish.  With the availability of lithium, I was able to drop that to 2 hours, start to finish!  Granted, this batch is MUCH smaller than what I used to make a long time ago.


Supplies:

3 24oz pop bottles
3 pint size mason jars
1 small container LYE crystals from hardware store
2 instant cold packs
2 Energizer Ultimate Lithium AA Batteries
2500 mg of Ephedrine HCL pills (or pseudo)
1 Container Coleman Fuel
24" Aquarium Hose
Aluminum Foil
Several ziplock baggies
Muriatic Acid
Epsom Salts
Acetone
ViseGrip plyers
Needle Nose Plyers
Coffee Grinder
Coffee Filters
Funnel
Latex Rubber Gloves


Procedure:

First off, for your pills, try and get single component pills, i.e. pseudoephedrine HCL as the only active ingredient.  Or, get a bunch of EPH (Ephedrine Hydrochloride) pills online, they are everywhere, I recommend getting them outside of the USA, check out Kaizen Ephedrine HCL pills, they are pretty inexpensive, and there are a ton of companies off the beaten path which will ship to the USA.  I am absolutely sure that this reaction will work for domestic pseudo, but try and make sure it doesn't contain Guaifenesin.

Clean out both bottles and all three jars and dry them completely, there must be no water at all in one bottle in particular, this “dry” bottle will be the reaction vessel.  If the others have a very small amount of water this is fine.  I recommend using a hair dryer to fully dry all bottles and jars.  In the coffee grinder place the ammonium nitrate balls from both cold packs.  Grind them up, and place powder in ziplock.  Grind up the ephedrine pills and put the powder into a ziplock.  If your lye is not the consistency of sand, put it in the grinder and grind it into powder and put that into a ziplock.  I used 100% lye crystals from the hardware store and didn't have to grind it since it was just like fine sand.  Clean your work area.  This reaction releases a lot of ammonia gas, so I recommend doing it in a well ventilated area.  I recommend setting up a fan in the room.

Prep the acetone bottle:

Put 1 cup of Epsom salts into the oven and bake at 415 deg F for one hour on a baking sheet.  Place Epsom salts into one of the 24 ounce bottles.  Add two cups of acetone to the same bottle, and tighten the cap as much as possible, then shake vigorously.  Let the bottle sit for 30 minutes, shaking every 5 minutes.  You now have created dry acetone.  Now you must filter out the salts, to do this, you simply use 3 coffee filters and filter out the acetone into a mason jar.  This is easy since you simply push down slightly on the filters covering the top of a jar and create a slight cone, then you filter the acetone.  This must be done quickly to keep the dry acetone from absorbing humidity from the air and from evaporating.  Give the bottle a quick wash with a little Coleman Fuel removing all Epsom Salts, now quickly put the acetone back into the 24oz bottle.

Another option is to use a wash bottle, or make a homemade one.      I have a wide mouth wash bottle which I used for this.  It looks like one of these:



If you want to, you can make one by taking a 12" piece of Aquarium Tubing and drilling a hole into a 24oz bottle and sticking the tube all the way into the bottle.  This way, when you squeeze the bottle, the acetone will flow out the end of the tube.  This is almost identical to the hydrochloride gas bottle, except that the tubing goes to the bottom of the bottle instead of stopping 2" in.

Put on Latex Rubber Gloves

Prep the lithium strips:

1) Go to Youtube and look up the video on "Get lithium from energizer battery"
2) Be very careful not to short out the batteries.  If you bend the side metal down on top of the anode, you can literally lock in a short and blow the battery.  If you occasionally see some tiny sparks, don't worry about it, you only completely ruin the battery if you accidentally bend some of the casing metal so that it is touching the anode in the center of the top of the battery, thus, shorting it out fast.  Watch the video.  Except for getting off the anode cap, follow the directions in the video.  The video says these batteries are built like fortresses and they are.  In the first step of the video the guy took needle nose pliers and fidgeted around with the anode cap for a few minutes and got it to come off, after the plastic wrapper, this is the first thing you remove.  It’s a major pain in the ass, but, it’s easy with visegrips (I tried for 10 minutes with the needle nose, no luck at all).  Lock the grips entirely so there is no gap, then clamp down on the anode and rip it off.  If you just use the pliers like in the video, it’ll take you forever.  Once the cap is off, use the needle nose pliers to tear down the metallic sides, and then pull out the washer, gas valve, and finally the battery core and place both cores into an airtight ziplock.

Prep Hydrochloride Gas Bottle:

1) Take one of the bottles and drill a hole in the lid which is slightly smaller than the aquarium tube.
2) Pull the Aquarium Tubing into the hole about 2 inches.  Make sure it is snug.  The idea here is that we are going to make Hydrochloride Gas in the bottle, it’ll travel along the tubing and we bubble the reaction with the gas to produce the meth hydrochloride salt.  This gas is toxic so we want to make sure that the tube is snug in the bottle.

Whatever you do, do not add water to this.  I don’t care what you’ve read, don’t do it.  There is no need:

NH4NO3 + NaOH ---> NH3 + NaNO3 + H20

This reaction releases a bit of water into the reaction chamber.  Now, maybe someone can tell me this, I thought that with the lithium/anhydrous ammonia reduction, that electrons were removed by water in the reaction chamber, if this is true, than why does the reaction work so well, given that the ammonia gas reaction is providing water in the reaction chamber?  Any answers are appreciated…

Begin reaction (use funnel to put chems into bottle):

1) Put 4 tablespoons of Ammonium Nitrate powder into dry bottle.
2) Put 4 tablespoons of Lye crystals into dry bottle.
3) Let sit for one minute, then with your hand, waft the top of the bottle and see if you smell ammonia gas.  This test will ensure you have the right chems in the bottle.  Some cold packs do not use ammonium nitrate.  This also builds up ammonia atmosphere in bottle for safety.
4) Add 12 fl oz. of Coleman Fuel
5) Do this part as quickly as possible since lithium metal will heat up a little bit, especially if the room is humid.  Open baggie with battery cores, and take them out.  Unroll each one and remove the lithium metal strip and set it down on a dry surface.  Quickly, pick up each strip and tear it into small strips placing the strips into the reaction vessel.  Do not touch the strips to other metal.
6) Pour in baggie full of crushed pills and put on cap.

Hold the container, and wait a few seconds and slightly loosen the cap so that ammonia gas can escape.  Now the reaction container should have the strips floating on top and you should see bubbles coming up from the bottom, this is ammonia gas.  To minimize the gas release, keep the lid tight until you feel the bottle tighten, then vent the gas slowly.  Do this over and over again for 60 minutes.  At 60 minutes, you will see small copper colored BBS floating on the top of the mixture, this is a good sign the reaction is complete.

Loosen the seal on the bottle slightly to let excess gas escape and sit it on the ground.

Take 3 coffee filters and place them over the opening to one of the pint jars.  Push down with your finger to make a cone shape in the jar with the filters over the top.  Pick up the reaction bottle and uncap it.  Slowly pour the liquid into the filters making sure to decant it so that none of the hard materials inside the bottle make it into the filters.  Some will, but this is not a problem.
Once the filtering is complete let the pint jar with the clear liquid sit for 2 minutes.  Check the bottom of the jar and look for any white or off white particles.  If you see some, decant the fluid into the second jar leaving behind all particles in the first jar.  Check the second jar after 2 minutes to make sure you got out all the solids.  If not, clean the first jar and decant again, the goal is to have a jar with just clear liquid in it.

Hydrochloride Gas to create meth crystals:

Now for the hydrochloride gas.  The most important thing here is to not add too much acid or foil.  The second most important thing is that when the gas stops flowing out of the bottle, the heat from the reaction dissipates and creates a vacuum inside the bottle, this is a little risky since the vacuum created can very easily draw fluid from the reaction backwards through the tubing and into the gas bottle.  If this happens, immediately dump the contents of the gas bottle, wash with water, dry and start over.

Safety Note: Keep a small bottle of water handy, such as a 24 fl oz bottle.  If the reaction goes out of control and you think it'll melt the plastic bottle, simply dump in the bottle of water and everything will stop.  It's a quick and dirty solution to a runaway reaction.

Open the gas bottle with the tube in it, and put in about 5-7 drops (NO MORE!!!) of muriatic acid.  Then, using the aluminum foil, tear off a small piece and roll it into a ball ½” inch in diameter and place it into the bottle, tightening the lid right after you put it in.  Now, sit the bottle down on the table and put the end of the tubing just under the surface of the liquid.  After about 30 seconds, the acid will start reacting with the aluminum and start pumping hydrochloride gas into the mason jar.  You will literally see what looks like snow appear in the jar.  This is raw meth.  Keep bubbling gas until the aluminum ball is completely dissolved, or the gas stops.  You can squeeze the bottle to push out more gas into the mixture, but be sure not to suck up any of the reaction, so after squeezing, pull the hose up out of the mixture when you loosen your grip on the bottle.  After the aluminum ball is dissolved, there should be a significant amount of meth floating in the jar as well as hydrochloride gas sitting above the solvent line.  If the gassing process didn't last at least 2-3 minutes, you can add another aluminum ball and a couple drops of acid to continue gassing.  You can now manually blow away the “smoke” or hydrochloride gas which is sitting on top of your mixture, do NOT breath in this gas, just exhale over the jar to blow away the gas.  Dry HCL Gas quickly adheres to water in the air and forms “smoke”, so this is what you are seeing.  Let the mixture sit perfectly still for 5 minutes.

Now most of the meth has settled on the bottom.  Put 2 coffee filters in the funnel, place it in the reaction bottle, and decant the mixture back into the reaction bottle.  We are going to do a second reaction.  After most to all of the mixture is back in the reaction bottle, take the 2 coffee filters and place them aside since these have meth on them.  Add one teaspoon of Ammonium Nitrate and one teaspoon of Lye to the reaction bottle and screw on the cap.

Doing exactly as before, loosen the cap when the bottle gets tight, and keep doing this for 30 minutes.  Afterwards, you can use the same three dirty filters you used the first time and decant the liquid into the third mason jar.  Loosen the cap on the reaction bottle and place the bottle on the floor.

Let the liquid sit for 2 minutes, and if you see solids at the bottom of the jar, decant the fluid into the jar which has the meth in it.  NOTE: To be extra safe, if you are decanting because of solids, it is better to first decant into a clean jar, then once you are sure the fluid in the jar is perfectly clear, go ahead and put the mixture back into the meth jar.  If you don’t see any solids, go ahead and pour it back into the jar with the meth in it.

Add 5-8 drops muriatic acid to the bottle with the tube.  Add ½” ball of aluminum foil to the bottle, and place the other end of the tube just under the surface of the liquid.  Now we are trying a second time to produce the hydrochloride salt of meth in the same mason jar which already has meth in it.  After the aluminum ball is dissolved, let the meth settle on the bottom again.

After 10 minutes, decant off the liquid into one of the other mason jars.  You now have a jar with about 2 grams of somewhat pure meth.  You now grab the 2 coffee filters used to filter the meth mixture you set aside earlier.  These filters have a lot of meth on them, so we are going to use them again.  Put these filters over one of the unused or dirty mason jars sitting on the table.  Again, push down with your finger to make an indentation in the filters like a small cone.  Take the acetone bottle and pour in a small amount of dry acetone into the meth crystals and swirl around the mason jar mixing the meth into the acetone, and cleaning it.  Quickly pour the mixture into the filter setup using the meth filters.  After the fluid is gone, you have pure meth in the filters.  You can add another splash of acetone to the filters to further clean your product.  After all the acetone is gone from the filters, remove the filters and sit them in an open air environment to dry.  You now have pure meth, pure white, around 2 grams, very high quality, sitting in the filters.

There will be a small amount of meth stuck in the filters.  You can remove the dried meth from the filters and then drizzle some water through the filters collecting it on a mirror.  Let it evaporate and crystals will form from the meth stuck in the filters.  Or, you can use the filters to brew a pot of coffee and it will have a nice kick.

You will immediately see that this meth is a very fine perfectly white powder.  Do not worry about this.  If you want to have huge crystals of meth, you can do a basic recrystallization process and this will give you big crystals instead of fine powder.  If you have questions on how to do this, lemme know, otherwise I'm sure there is a ton of info here on how to do that.  Enjoy!

Disposal:

Let the reaction vessel sit with the cap loose overnight before disposing of it.  Throw out the battery components, the reaction vessel, take apart the smoke bottle and clean it, clean everything.  Make sure you put your lye under your sink, cold packs in the medicine cabinet.  BE SMART, leave no evidence.  Throw away your stuff all over town in different trash cans in different places.  Wipe off prints off your vessel, etc.  Toss the filters, BE SMART!


Please ask away if you have any questions about the procedure, this is a very simple procedure and with the cost of pills being reasonable, this is definitely the way to go for personal/occasional use.  For bulk I would recommend a different procedure. " -dkmonk

What's the average yield from this out of interest?
Title: Re: Chemistry Discussion
Post by: dkmonk on August 14, 2012, 12:52 am
If you have 3 grams of pseudo you will get about 2.5 back once you add in loss from the filter and whatever is stuck to the jars and plate. New people doing this will have lesser yields due to inexperience, but as long as you are getting over half of what you put in back then I would say you did alright for a beginner.

I will be adding comments about this method throughout this post as there is a big thread that I was a part of that had many good suggestions, that are definitely not necessary, but if you are really trying to do it in the best possible way could help.

 
Title: Re: Chemistry Discussion
Post by: dkmonk on August 14, 2012, 01:08 am
All of this is related to the post that Mashman posted from me. I will designate the beginning of a different post by a - 

-On a another note, I was doing some afterthought on the reaction and knowing how bad it is to have water in the solution for many reasons, not just the Li+H20 reaction, but, mainly because of the high level of solubility of meth hcl in H20. Anyway, since the ammonia reaction,

NH4NO3 + NaOH ---> NH3 + NaNO3 + H20

Produces water as a byproduct, this will result in less yield when gassing the solution since H20 will be present in the solvent.  I was thinking of making a few changes to make sure there is absolutely zero water in the final solvent.  Please let me know what you think of these changes...

1)  First, we would base the PSE/EPH with NaOH + H20 + Toluene.  We wash the filter cake with 20-30 ml's of water.  Then using a sep funnel we separate the toluene and water layers.  We then wash the Toluene with 50 mls of water and separate again.  After separation, we add anhydrous MgSO4 to the toluene to remove any residual water.  (This is theoretical since I know there have been many filler advancements made with polymers)

2) We add Toluene to the solution until we have the needed 12 fl. oz., Toluene is very non-polar.  In my opinion, I think a 100% toluene solvent would result in a cleaner product.

3) By removing most of the fillers, we will have a faster reaction since there will only be EPH/PSE base, some non-polar soluble fillers, and our NH4NO3 and NaOH.  This will allow the NH4NO3 and NaOH to react more quickly because there won't be an equal volume of filler solids in the reaction vessel.  Otherwise, with my original post, there is so much filler solids in the reaction vessel, it requires frequent agitation to keep the reaction going.

4) After the reaction is complete, we filter the solvent into a jar.  The water layer from the reaction will likely not be visible since the amount produced will be small, however, to prevent loss, we dry the solvent with a few grams of anhydrous MgSO4.  The solvent is then filtered again, and afterward a few ml's of Toluene is added to the remaining MgSO4 and filtered into the main solvent basin.

5) Now, first off, the HCL + Al reaction I posted before to make HCL gas is a no no.  The reason being that the only reason HCL gas is released is because of the  2Al + 6HCl ---> 2AlCl3 + 3H2 reaction being exothermic, this boiling the HCL(aq) to produce HCL gas and evaporated H20.  The other obvious problem here is that we get H2 as a byproduct which in off itself is dangerous to some degree, and we'll end up having H20 in our solvent, likely bound to the Ammonium Chloride formed.  So, to replace that step, we go with HCL(ag) injected into a small port on our gas bottle which contains 1/2 cup of H2SO4 (Sulfuric Acid Drain cleaner).  We just inject a few drops and the resultant reaction makes HCL gas.  Now, to further ensure we are not introducing water into the solution, we can rig up a second bottle in the following way.  The hose from the gas bottle is lengthened and ran through the top of a second bottle until it is touching the bottom of the second bottle.  The second bottle has 2 holes drilled into the top.  One hole for the hose from the gas bottle, and one for a hose which extends only one inch into the bottle.  The idea is that we take the gas generated by the gas bottle and filter it with the second bottle.  In the second bottle we fill it half way with anhydrous MgSO4 to remove any water vapor in the HCL gas since it is very hygroscopic.  Another option would be to bubble the HCL gas through H2SO4 in the second bottle since it too is very hygroscopic.  Anyway, the whole idea here is to make anhydrous HCL gas.

So, the changes made to the original process are basic, we use a different non-polar solvent, Toluene.  We base the EPH/PSE first and remove most of the solid fillers, we dry the resultant reaction, we make anhydrous HCL gas, and this should result in the highest precipitate.

The one thing I like most about this reaction is that there are very little impurities compared with the Red Phos, Iodine reduction.  So many things go wrong with that in my opinion.  Just the iodo-meth byproduct itself is impossible to get rid of when present, not to mention all the other dangers.  The NH3 Lithium reduction produces very little byproducts.  The lithium amide produced is destroyed by the H20 from the NH3 making process.  The only other possible contaminant is Ammonium Chloride, which is from the NH3 in Solution with the Toluene and the HCL Gas, HCL + NH3 ---> NH4CL.  However if one lets the solvent sit for awhile, most of the NH3 will evaporate and you will have a negligible amount of NH4CL.  Also, when you gas the solvent, most of the NH4CL formed will remain in solution in stasis, so in reality, if you decant it right away, I doubt any would remain in the solute.  Plus, if you absolutely wanted to make sure there was no NH4CL in the final product, an A/B re-crystallization would ensure that, since NH4CL + NaOH = NH3 + NaCL + H20, so if it were present, it would be destroyed.  So, all in all, I think this process is a far cleaner and safer process than the other PSE/EPH methods.

- My write up was meant for the layman, while my second post about improving the process was meant to be more technical since the issue of having water in the final solution, and having water in the gas you use in that solution, could potentially lead to degradation in yield.

The concentrated sulfuric acid one buys at the hardware store is pretty strong, usually about ~96%, but, it's weaker than HCl.

I wanted to make an addition to my last post, I wanted to say, add a solution of HCl AND NaCl via a syringe to the H2SO4.  Since muriatic acid is only ~30% or so, when you push on the syringe and inject the muriatic acid + NaCl solution, you would have an HCl Gas release from the HCl(aq) + H2SO4(aq) combination which would be exothermic, and a release from the NaCl + H2SO4 reaction.  Since the NaCl + H2SO4 reaction releases little pressure, I thought that if we added HCl to the mix, we would get some pressure to push the gas through the second chamber which dries the gas.

The only issue is see with this is how much NaCl can we realistically dilute the Hcl with?  That I don't know, but, I would imagine not much.  In any case, if we can't mix in the NaCl, the H2SO4 + HCl reaction works perfectly.

Even with anhydrous Sulfuric Acid, we will still have water vapor in the gas.  If we go with just NaCl and H2SO4, the water vapor will be minimal but the reaction is very slow and it's very messy.  The reaction: H2SO4 + NaCl --> HCl(g) + NaHSO4 releases minimal HCl gas compared to H2SO4(aq) + HCl(aq) --> H2SO4(aq) + HCL(g).  The addition of NaCl in solution with the HCl was to take advantage of the extra minimal reaction since it wouldn't hurt the primary reaction at all.

We can dry the gas 2 ways, either by bubbling through H2SO4 (which may be the best method), or by bubbling through a drying agent such as MgSO4.  To make things very easy, and since the Sulfuric Acid available is very strong, I would think simply bubbling the gas through the H2SO4 would make the most sense, since we wouldn't have to bake the Epsom Salts, and then crumble them up and stuff them down a funnel into our second bottle.  Strong H2SO4 is very hygroscopic, it will definitely dry the gas, ensuring it is anhydrous.

Then for the second issue, water in the reaction vessel from the NH3 (Ammonia Gas) production, if we dry that with a couple grams of Epsom Salts (MgSO4), we will make the solvent mix anhydrous before gassing procedure.



-A few pointers: I would recommend chilling the reaction bottle on an ice/brine bath and displacing all air in the bottle with argon before adding lithium to it, otherwise KA-f-ing-boom is definitely possible if you have too much H20 in there. Moisture from the air should be sufficient to start the ammonia generation reaction, so no water would be needed. Would definitely purify end product with a final AB workup too, lithium is not too good to smoke!



- The double bottle gas method gives about a 20% increase in yield.  I took 2 bottles, around 20Fl Oz, with a wide mouth.

I filled one half way with sulfuric acid, the other 1/4 way with muriatic acid.

I drilled 2 holes in the lid with the sulfuric acid small enough that the aquarium tubing was snug.  I drilled one hole for the tube and a very small hole for the syringe in the muriatic bottle.

After cutting 2 pieces of tubing, I ran one from the top of the muriatic acid bottle to the bottom of the sulfuric acid bottle.  I then ran the other from the top of the sulfuric bottle to the solution to be gassed with HCL.

I filled up a syringe with sulfuric acid and pressed it against the muriatic bottle lid to make it snug and sealed.

Literally, as I pushed the plunger the gas bubbled through the sulfuric and out the top through the tube into my solvent.  It was completely dry, and I got the largest yield yet!

I'm used to using sulfuric and salt and it's a pain in the ass since it;s so slow and takes so long.  With this, I was done in seconds.  As soon as you push the plunger, gas starts flowing and bubbling, there is no steam at all, it's completely dry.

Worked awesome!  Blows away salt method.  In the past, I always had some residue which I always thought was from the coleman.  But it was water in the solution, I know because this time there was nothing left at all, my yield was amazing.



- The over-reduction of EPH/PSE results in not only the Hydroxyl (OH) group being reduced, but the aromatic ring as well.  When the aromatic ring is reduced, EPH/PSE is reduced to CMP, 1-(1′,4′-cyclohexadienyl)-2-methylaminopropane.  Also, if you read that document, the percentages are really high in some cases, especially when using non filtered pills as a starting material.  Now, the number one contributor to CMP's presence in the final product is the presence of an aproton material, namely water.  So, if water isn't present, this greatly reduces the chances that CMP will be in the final product.  Also, the document speculates that the excipients in pills act as catalysts to produce CMP, I disagree with this, I think that this is from moisture in the excipients since most of them are very hygroscopic.  The solution here is to minimize water and use about 1/4 strip of an Energizer AA Ultimate Lithium for 2.5grms PSE.  This is a close stoc. measurement.  The actual stoc. is 2:1 li:pse.

Now, to be extra safe, I recommend a 3% potassium permanganate KMnO4 wash to break the bonds in CMP.  Since you should do an A/B extraction anyway, this can be added to that, simple dissolve product in 3% KMnO4 solution, then add lye to freebase the meth, than add Xylene/Toluene to dissolve the freebase, then separate the solvent from the KMnO4 solution and dry the solvent with baked MgSO4 and gas with dry HCL.  This will get rid of any and all possible impurities including lithium, lithium amide, lithium bronze, various salts, etc.  Then you could recrystallize in hot Iso with an acetone flash.


As far as answers to a couple of your questions...


Anyways, what is happening in the lithium/ammonia reaction is that the EPH/PSE is being hydrogenated.  The only difference between ephedrine and meth is that ephedrine has an extra hydroxyl group.  This reaction reduces that group to form meth.  It is a 2 step process.  Check out online references to Birch Reduction.

As far as gassing, what that does is pretty simple.  The meth freebase is soluble in solvents such as camper fuel.  However, meth HCL, is NOT soluble.  So, when you gas the solvent with HCL gas, the HCL Salt of meth is formed which is NOT soluble in solvent, and thus it precipitates and falls to the bottom like snow.


- This is a link to "Birch by product and Yields"
http://txn.fd.org/Bremer%20Meth%20Yield%20Report.pdf



- NH4NO3 + NaOH ---> NH3 + NaNO3 + H20

The above is what produces the Ammonia gas which dissolves the lithium into solution.  Ammonia liquifies under a small amount of pressure so you will notice that if you let some pressure build up in the bottle, then loosen the cap, the liquid ammonia will quickly boil off.

The only problem with this reaction is that water is produced.  Therefore, you will have mixture of base meth in solvent and water.  When you gas the mixture, meth crystals from in the jar or whatever you filtered your mixture into.  Now, since the hydrochloride salt is soluble in water, I'm sure there is some loss of yield because of this.

My thinking is that if you use something different from Coleman fuel, such as toluene, you will have better yield since you can let the filtered solution sit and using a sep funnel, or something similar, you can separate the toluene and water BEFORE adding HCL gas.  Or,
NH4NO3 + H20 -->  NH4+(aq) + NO3-(aq) + H20
NaOH + H2O ---> Na+(aq) + OH-(aq) + H2O

Then you get:
NH4+ + OH- ---> NH3 + H20
and
Na+ + NO3- ---> NaNO3

Therefore, for the reaction to happen, water in the air, or water present in the Sodium Hydroxide/Ammonium Nitrate is what starts the reaction.  Once the reaction begins, more water is produced, thus, the longer you let the reaction happen, the more water is produced.  I noticed the second time I tried the reaction, I let it go much longer since it was slow starting and I had less yield.

So, there must be a valid solution for this, even though I don't plan on doing this again for a long long time, I am curious about it.  I've thought about ether as well, but it's just too hard to get clean ether.  So, is toluene the best bet?

Or what about adding a few grams of Magnesium Sulfate to the solution before gassing, then decanting it or using a vacuum filter.  Will the Magnesium Sulfate just soak up the water, or is there a risk it will adhere to some of the end product?

Also, what about washing the Coleman Fuel with toluene, or xylene?  Will this capture the freebase?  Anyway, I appreciate any answers to this perplexing problem, I'm not exactly sure how much water is produced, but I bet there is definitely some loss because of this.

I was thinking a little bit more about this and I bet the best way to do this reaction is to first freebase the PSE/EPH in toluene, and use that as the solvent.

Then after the reaction, you would let the solution sit for an hour or so, and use a sep funnel to remove the water layer, then dry the toluene afterwards with MGSO4.

The only part I'm unsure on is the solubility of NH3 in Toluene.  I would imagine it would work fine, thoughts?


Title: Re: Chemistry Discussion
Post by: Rawkingfish on August 14, 2012, 01:49 am
Fantastic post dkmonk! I only skimmed, as I'm currently contending with the in-laws stopping by for a surprise visit :( But this thread is a great idea.
Title: Re: Chemistry Discussion
Post by: EzzeeK on August 14, 2012, 02:02 am
Awesome thread,  I have a shit load of 30mg adderall and want to make Ice.  I"m new to cooking,  Are cold pills better or can I skip some steps with adderall?
Title: Re: Chemistry Discussion
Post by: dkmonk on August 14, 2012, 02:09 am
Just sell your Adderall and then you will have a shit load of money and can make way more meth than you will get out of those pills. For about 50 dollars you can make a few grams of meth.

Title: Re: Chemistry Discussion
Post by: EzzeeK on August 14, 2012, 02:16 am
I could only sell them for $5 a piece locally and I don't know if I want to make an account.   I just want to know if I can make Ice cheaply with adderall without a lot of overhead?   
Title: Re: Chemistry Discussion
Post by: jimbeeno320 on August 14, 2012, 02:56 am
hey gonna try this and let ya know how it goes. will be my first time and will take precaution(wear gloves, mask, work outside) but the only part i have a question on is how much aluminum, you say a small strip 1/2" but how wide? like the size of a finger or so?
Title: Re: Chemistry Discussion
Post by: jimbeeno320 on August 14, 2012, 03:29 am
also, heres some help with condensing ammonia on rhodium/erowid

http://www.erowid.org/archive/rhodium/chemistry/birch.mrclean.html

i'm facinated with chemistry
Title: Re: Chemistry Discussion
Post by: dkmonk on August 14, 2012, 04:37 am
hey gonna try this and let ya know how it goes. will be my first time and will take precaution(wear gloves, mask, work outside) but the only part i have a question on is how much aluminum, you say a small strip 1/2" but how wide? like the size of a finger or so?

Read all the other posts that I put, because there is a way without alluminum to use as the smoker. You can get sulfuric acid (liquid fire is a brand) and then use salt instead of aluminum and muratic. Just fill the bottom of your vessel with about an inch or half inch of salt then with gloves and a funnel pour in your sulfuric acid slowly until it starts smoking and foaming. Don't pour a lot or do it too fast because the reaction will make it foam over and out your tube. You don't want this on your skin it hurts.

If you read everything I posted you will see how the thread went from the first post, and then the ideas and changes we suggested to tweak the original and refine it. The original will work very well, but we just nit picked it to make it safer and better yield. Here is the part that you would of read that contains to your question if you completely read my other post.


5) Now, first off, the HCL + Al reaction I posted before to make HCL gas is a no no.  The reason being that the only reason HCL gas is released is because of the  2Al + 6HCl ---> 2AlCl3 + 3H2 reaction being exothermic, this boiling the HCL(aq) to produce HCL gas and evaporated H20.  The other obvious problem here is that we get H2 as a byproduct which in off itself is dangerous to some degree, and we'll end up having H20 in our solvent, likely bound to the Ammonium Chloride formed.  So, to replace that step, we go with HCL(ag) injected into a small port on our gas bottle which contains 1/2 cup of H2SO4 (Sulfuric Acid Drain cleaner).  We just inject a few drops and the resultant reaction makes HCL gas.  Now, to further ensure we are not introducing water into the solution, we can rig up a second bottle in the following way.  The hose from the gas bottle is lengthened and ran through the top of a second bottle until it is touching the bottom of the second bottle.  The second bottle has 2 holes drilled into the top.  One hole for the hose from the gas bottle, and one for a hose which extends only one inch into the bottle.  The idea is that we take the gas generated by the gas bottle and filter it with the second bottle.  In the second bottle we fill it half way with anhydrous MgSO4 to remove any water vapor in the HCL gas since it is very hygroscopic.  Another option would be to bubble the HCL gas through H2SO4 in the second bottle since it too is very hygroscopic.  Anyway, the whole idea here is to make anhydrous HCL gas.
Title: Re: Chemistry Discussion
Post by: dkmonk on August 14, 2012, 04:42 am
You should be able to make meth pretty easily from amphetamine. I have never done it or looked up the process, but it is possible and wouldn't be intensive. I just don't see the reason because it would take 100 of your pills and you won't even get 3 grams out of it. It just doesn't seem worth it at all when psuedo costs less than 10 bucks for 3 grams at the pharmacy and your supplies maybe and addition 30 bucks.
Title: Re: Chemistry Discussion
Post by: john_snow_da_bastard on August 14, 2012, 05:08 am
dkmonk, thank you for sharing this.

How much odor does this put off? Is it restricted to the boonies or can it possibly be done without tipping off the whole block?

In either case, in your your experience was this a strict outdoor activity?

This seems so much safer (and I say that cautiously) than some of the other 1 pot approaches I've seen.
Title: Re: Chemistry Discussion
Post by: dkmonk on August 14, 2012, 05:18 am
The smell of anhydrous is strong, but it dissipates really well. I feel safer doing it inside with a fan or two and a window open that doesn't point directly at a neighbors house. In a garage is perfect, with a fan too.

Just be smart and don't do it in a motel or something like a lot of idiots do. That is about the equivalent of doing it in your neighbors backyard.

I don't like doing it outside, because it is open for anyone to walk up on you or see your car randomly parked some place with nobody in it and get suspicious. There is also the humidity that comes into play from being outside and you don't want high humidity it not only lowers your yield, but also makes it less safe.

As long as you don't live in an apartment you are fine doing it indoors with good ventilation. I would recommend a mask or respirator because no matter what you will definitely smell it yourself being right in front of it and it a good whiff of ammonia right up the nose is enough to make take your breath away.
Title: Re: Chemistry Discussion
Post by: Operation Shulgin on August 14, 2012, 12:34 pm
Hey shulgin, I would love a chem section and I wish there were more precursor classifieds...I have a lot of info to contribute but also would like pointers and some advice on some reactions as well.

I guess we are in the same boat! I'd loveto see a chemistry section and wish there were more (non overpriced) precursors available, but i'm confident that we can make this work!

Great to see the input my anonymous friends, you have no idea how big the smile on my face is! /Not telling you because of LE (just kidding :) )
I hope this thread grows and stays on topic and if the mods like it we might get our selves a chemistry section on the forums!

Organic/underground chemists make yourself at home and grab a drink!

Cheers, Operation Shulgin!
Title: Re: Chemistry Discussion
Post by: Dark Moon on August 14, 2012, 04:56 pm
Nice another thread to keep up with. I like the subject. Nice posts dkmonk. Let's keep this thread alive! :)
Title: Re: Chemistry Discussion
Post by: Rawkingfish on August 14, 2012, 06:42 pm
This thread is making me stare at my Sassafras trees behind the house....giving me ideas I shouldn't be having. I know the safrole content is fairly low....but the part of me that likes projects gets all excited at the thought of setting up some glassware...

One can dream.

 
Title: Re: Chemistry Discussion
Post by: rubixcoffin on August 14, 2012, 08:19 pm
the partial archive of rhodium over at erowid is certainly a very decent resource! i've "perused" it many times myself, all sorts of useful stuff :)
was gonna suggest it myself! but glad others got there first :D
Title: Re: Chemistry Discussion
Post by: jimbeeno320 on August 15, 2012, 02:41 am
yeah on mr clean's site he states magnesuium shouldnt be used to dry ammonia but i dunno if that applies here. if you've tested it i'll take your word for it
anyway i asked erowid and....
http://www.erowid.org/archive/rhodium/chemistry/hclgas.argox.html
not that i'd ever have all that equipment but it shows the pros and cons and a couple different techniques
sorry if i'm just rehashing whats easily accessible out there

so yeah, gonna go with the salt/sulfur route, cleaning up my pfed first with the waterless a/b tek on rhodium. i'll let y'all know how it goes

eventually i want to build my confidence up, invest in an ammonia generator and mess around with some micro birch reductions

wouldn't mind doin a kerosene/sulfuric extract on the coca leaves on here either,  oxidize with some potassium permanganate and base it up, vendor seems kinda iffy though(extractions are my strong point, my evil twin used to do bulk dmt extractions)

oh and hola dark moon! glad to see ya.
^(great vendor)


Title: Re: Chemistry Discussion
Post by: jimbeeno320 on August 18, 2012, 06:11 am
bright stars synthesis shows a 10% yeild from safrole so 10g if you have a reliable safrole source

http://www.erowid.org/archive/rhodium/chemistry/brightstar.mdma.html
Title: Re: Chemistry Discussion
Post by: john_snow_da_bastard on August 18, 2012, 06:37 am
@ dkmonk (or any others with actual experience with the modified birch rxn)

1. Have you ever witnessed a reaction vessel explode? Or the lithium react with water? I'm curious if in addition to safety gear, if the reaction steps could be carried out within something like a turkey bag, or homemade tupperware tub (clear) glovebox for an added layer of safety.

It's not clear to me if the horrific accidents and burns we all hear about are from.these bottles exploding are more similar to a shaken soda (shooting caustic solution instead of soda), or the explosions are more like an explosive.

In the former scenario the bag/box precaution seems useful, but probably futile in the case of later where there is.actual.combustiion.

Ive always wanted to try this but I cant bring myself to do it until i'm certain it wont involve 3' burns and disfigurement :)

My understanding is that aside from caustic injuries, lithium and water rxn & internal pressure of rxn vessels are the things to worry about in this synth.

2. Earlier this year I used Coleman's camping fuel in a DMT extraction. When I evaporated it to leave the freebase behind I discovered it contains a blue rust inhibitor.that totally fucked everything. Gassing with HCl should bypass this issue, but I'm skeptical of Coleman's and it also has an odor that lingers like a bitch.

Therefore Toluene seems more appropriate. Is it less odorous? And do.they still carry suitable versions at the hardware stores?

Thanks in.advance.
Title: Re: Chemistry Discussion
Post by: Pusci on August 18, 2012, 06:59 am
Im curious to how much safrole one would expect from say 100g of sassafras root bark ?
Title: Re: Chemistry Discussion
Post by: jimbeeno320 on August 18, 2012, 07:16 am
no idea really. somewhere on erowid said 10%. btw root bark on the road seems crazy expensive unless in reality it is some kind of extract. botanical shops have much lower prices on google that make the idea of actually going through all the work of distillation and reaction worthwhile.

lb rootbark $30 (google)-  45 g safrole x 3 - 150 g
90 bucks theoretically to get enough for half oz plus regents glassware ect. 
Title: Re: Chemistry Discussion
Post by: le botbahn on August 20, 2012, 06:24 pm
Bump. For science.
Title: Re: Chemistry Discussion
Post by: Tsjanga on August 26, 2012, 04:51 pm
Anyone tried the TCCA route for amine to amide?
Title: Re: Chemistry Discussion
Post by: DiscountDank on September 12, 2012, 08:58 pm
Hey is there any reliable way to wash MDMA/MDA hcl or sublimate to purify?  I have a chemglass sublimator (i think its a sublimator), its a glass apparatus which looks like it has in/out for cooling and you are supposed to put your hcl in a bottom part of the apparatus and then it is supposed to transport and attach when it is purified to the upper piece.  I dont think its under vacuum, but wanted to give it a try and see if and how the contraption works.
Title: Re: Chemistry Discussion
Post by: dkmonk on September 12, 2012, 10:00 pm
I am pretty sure you can wash MDMA just like meth or coke and it works just the same. Anhydrous acetone over the crystals and then filtered and dry. LeJunk said it is good for washing MDMA and he is the one who made washing coke with acetone popular, or at least he is referred to an awful lot for making it more known. Look up Lejunk and ecstacy wash. I am pretty sure he posted a thread about it after he posted his famous cocaine wash tek thread.
Title: Re: Chemistry Discussion
Post by: DiscountDank on September 12, 2012, 10:37 pm
thank you, washing is def a good way and it looks like a lot of vendors are washing their product, I want to see if I can successfuly sublimate hcl in my apparatus but cannot find any good instructions even on erowid.
Title: Re: Chemistry Discussion
Post by: Montell Williams on September 13, 2012, 01:08 am
Sublimation is when a material changes from a solid to a gas like iodine or benzoquinone. MDMA absolutely will not sublimate.
Title: Re: Chemistry Discussion
Post by: giantboyfriend on September 13, 2012, 01:54 am
I for one would love a chemistry section, also I have a question maybe someone here could answer in regards to MDMA.HCl

I have always used an HCL gas generator to precipitate my salts from freebase solution although another member on another forum suggested another method that seems much more preferable as HCL gassing is a mess and the clean up is no fun.

Extract freebase alg using xylene
drying xylene with drying agent(mgSO4)
combining equal parts of xylene/product with 99% IPA.
titrating IPA/xylene mixture to PH of 6 using 31% HCL solution
vacuum distill IPA off which should leave xylene and salt formed in flask
drying salt in a pyrex dish through evaporation then a little acetone at the end

I just wanted to verify before I try such method as it seems like a nice alternative to HCL gas.
Title: Re: Chemistry Discussion
Post by: DiscountDank on September 13, 2012, 02:00 am
Sublimation is when a material changes from a solid to a gas like iodine or benzoquinone. MDMA absolutely will not sublimate.

Are you sure I could have sworn there was a write up on sublimation on erowid and one synth directly mentioned that for perfect purity to sublimate your final mdma product, after washing it and separating it plus washing it through a freezer technique...
Title: Re: Chemistry Discussion
Post by: 34trimethoxy on September 13, 2012, 02:20 am
I'll be contributing to this.
Title: Re: Chemistry Discussion
Post by: Chapman on September 13, 2012, 02:40 am
+1 for chemistry section. 'twould be great.
Title: Re: Chemistry Discussion
Post by: shman on September 13, 2012, 04:02 am
+1 for chemistry section. 'twould be great.
make it +2
Title: Re: Chemistry Discussion
Post by: DrDeepWood on September 24, 2012, 01:27 am
Post your questions in here, I offer a professional chemistry consulting service on silk road under the name "ron paul"
If its a question which will apply to the community I will answer it here for free
Title: Re: Chemistry Discussion
Post by: chemdog on September 24, 2012, 11:45 am
Another vote for a chemistry section.

+100
Title: Re: Chemistry Discussion
Post by: The Red Hippogriff on September 25, 2012, 05:04 pm
I must say I dislike the idea of a chemistry section on the SR board. The .onion sites are slow enough as it is without bogging down the bandwidth with theoretical discussions. There are already plenty of sites on clearnet for that kind of thing, and they have a lot more stable connections. I'm not sure how the Dread Pirate keeps this service hosted now, it must cost a fortune, I can't imaging it would be a good business decision to increase traffic for non-customers.