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Discussion => Drug safety => Topic started by: yeababy on August 05, 2013, 05:46 pm

Title: RON PAUL SYNTHESIS FAILURE (Anhydride for fun and profit)
Post by: yeababy on August 05, 2013, 05:46 pm
After spending some money, taking some useless risks and failing miserably. I believe it is time to get some real conversations going on.

I wish this place could become more technical oriented. If someone has some real background and can teach me how to cook. Contact me. I am no time waster and i have money. You must be willing to accomodate to some conditions so dont waste your time trying to make a quick buck of me.

-if you have some chemistry background please do comment.
-Please dont post irrelevant stuff like " all the kids are gonna be baking at home" they wont....this not shake and bake stuff.
I fell for that marketing pitch, and this is way more complex than that.

Please do comment,
Regards.
Yeababy

Acetic Ahydride Synthesis:
You need sodium bisulfate, make sure its SULFATE not sulfide, it is used as an Acid ph up in pools.
Pour a 1/4" layer on a large pyrex and put it in an electric oven as close as possible to the heating elements.
Put the oven on broil and watch the powder.
It will start to melt and bubble, when it stops bubbling you are finished dehydrating it.
Another sign that its done is a white film will form ontop.
Let it sit in the oven until its cool, shit is dangerous molten hot!
Now break it up, put it into a bag and smash it to tiny peices.
Load this in your blender and get it a superfine powder.
Its a little pungent, dont breath it in.
Now add an equal part of calcium acetate and blend.
Load this into a flask with a distillation setup, acetic anhydride will distill over as the two powders react.
If the reaction slows down because the two powders cake in,
very carefully add water to about 10ml of acetic anhydride to turn it to acetic acid, then pour this into the powders, will help wet it.
Once all your anhydride is distilled over good luck cleaning the glassware out, that powder cakes in there like crazy,
best best is do consider it disposable and do big batches to make it worth your time.


Propanoic Anhydride Synthesis:
This synthesis is very much the same except you use calcium propanoate instead of calcium acetate.
For this reaction you do not need to "wet" it, just mix the two powders and distill off!


Acetylation parameters:


Usually during acetylation you just have your substrate, what you are acetylating, the anhydride and a solvent.
For a much faster reaction you can use sodium acetate as a catalyst.
This is the compound thats present in those re-usable heating pads, with the little metal disk you click to start the reaction.
This is also safe to ingest so you dont always have to worry about cleaning it out of your product. I would use 2% compared to your anhydride.
So 20g of anhydride and .4g sodium acetate.
For anhydride ratio to substrate you can use anywhere from 10x to 100x molar excess,
I read a paper saying that there is no real hard and fast rule.



di-proponyl morphine aka super heroin:

For this you need to buy morphine tabs, preferably instant release but im sure extended release will work too.
Grind them up and pour them in a hot water solution, stir until dissolved.
You need enough water to totally cover the pill mass about 2x. Shake/stir for 2 minutes.
filter the solution so there is nothing floating.
Now dissolve sodium hydroxide in a water solution 10g sodium hydroxide to 100ml water.
Add this sodium hydroxide solution to the morphine   mix a few drops at a time, checking with pH papers.
Your goal is 9.1-9.3pH, do not go above this! be careful, when it gets close just add a drop at a time.
Now at that pH put the solution in fridge overnight and your morphine freebase will precipitate out.
Filter and save this morphine freebase, put it out on a plate on the window until its dry.
Now dissolve that freebase in about 250ml of acetone.
 
Add 10ml propanoic anhydride and .2g sodium acetate, boil for 1 hour and either distill off the solvent or pour it on a pyrex dish and let it evaporate.
You may want to add a cutting agent like mannitol because the amount is so small.
10mg is very active



loperdamide opiate:

This is a strong opiate which is made from loperdamide, this can be found over the counter anywhere.
You need to find the smallest loperdamide pills possible because you will not be extracting them, so this means less filler.
Grind up the pills, keep in mind, after conversion, one pill will be about one dose. Now dissolve all your pill mass in acetone.
If you have about 200ml of pill powder, use about 500ml acetone.
Add 10g propanoic anhydride and .2g sodium acetate.
Now reflux this mixture for about 1 hour, 2 is better.
Remove the solvent either with a vacuum or by pouring the mix on a pyrex and letting it evaporate.
Be careful with this powder and start small! There is no point in extraction because the binders will not react with the anhydride and the amount of compound is so tiny.


propoxy ester THC:

This is my favorite. Extract 10g of pot with about 100ml of acetone, charge the acetone into a flask and add 1g of propanoic anhydride and .1g of sodium acetate (if you want a faster reaction).
Reflux for 1 hour with a catalyst or 4 hours without. Evaporate off all the solvent and collect the tar. This shit is strong! be careful! It feels so nice but there is a reason edgewood aresenal investigated it as a weapon! You can do this also by dissolving hash in acetone, just keep the thc to PA ratio the same, or around the same.

Superhash guide

First you need to make propanoic anhydride, you will need a large round bottom flask and a distillation adapter, as well as a heated sandbath.
You need sodium bisulfate, make sure its SULFATE not sulfide, it is used as an Acid ph up in pools. Pour a 1/4"-1/2" layer on a large pyrex and put it in an electric oven as close as possible to the heating elements. Put the oven on broil and watch the powder. It will start to melt and bubble, when it stops bubbling you are finished dehydrating it. Another sign that its done is a white film will form ontop. Let it sit in the oven until its cool, shit is dangerous molten hot! Now break it up, put it into a bag and smash it to tiny peices. Load this in your blender and get it a superfine powder. Its a little pungent, dont breath it in. Now add an equal part of calcium propionate and blend. Load this into a flask with a distillation setup, and set it up to heat on a sandbath. Increase the heat and propanoic anhydride will distill over as the two powders react. It will start off slow but soon a liquid will distill from the two powders. 2kg of mixed powder will make around 250-400ml of propanoic anhydride, a very large amount. Store this in a flask with a sealed lid. If you need to scale up this synthesis make a large stainless steel can with a tube coming from the top, this tube must be cooled and let drip into a collecting bucket. Around the can place a flexible heating wire and insulate with fiberglass to keep the heat in.


Now we will turn the hash into hash oil and also react it with the propanoic anhydride at the same time. For every 20g of hash use 100ml of acetone, break up the hash into tiny peices and let soak in the hash overnight, make sure to stir or shake. Pour the green liquid through a filter to remove anything that did not dissolve. Now you have an acetone solution which contains THC/oil. Add 5ml propanoic anhydride for every 100ml of hash/acetone solution, and add .1g of sodium acetate (found in those click-bag reusable heating pads). Pour this solution into a round bottom flask and boil for 2 hours, include a reflux condensor from your distillation setup so vapors do not spread. Once it is boiled off either distill off the acetone with distillation setup or just evaporate in the open. Do not totally evaporate, leave it as a thick liquid, maybe like maple syrup.
This needs to be mixed with a large amount of hash, 10-20ml of this liquid will be added to 1kg hash. To add it to the hash break up the 1kg hash and coat with minimal amount of acetone, so it is a thick paste, then add superoil liquid and mix together very well. Spread hash on a pan and let acetone evaporate, better outside. Once it is a solid again break it up and repress it into bricks using a hydraulic press and mold.
Title: Re: RON PAUL SYNTHESIS FAILURE (Anhydride for fun and profit)
Post by: snstmission on August 05, 2013, 06:45 pm
Where did you fail?
Title: Re: RON PAUL SYNTHESIS FAILURE (Anhydride for fun and profit)
Post by: Ben on August 06, 2013, 01:22 am
It seems you are dunking a lot of processes for working on different substances here in one post. I do have a degree in chemistry, but if you want any real feedback, please be specific about which reaction you want to perform.

I'm glad to help you with any specific process, but please choose what you want to do before asking, and google whatever you can find first. If you have any practical questions on how to proceed after that i'd be happy to help out.
Title: Re: RON PAUL SYNTHESIS FAILURE (Anhydride for fun and profit)
Post by: HCeline on August 06, 2013, 04:23 am
Is that what he was selling for that Anhydrides for fun and profit synth?  wow.  I pm'd you
Title: Re: RON PAUL SYNTHESIS FAILURE (Anhydride for fun and profit)
Post by: hoobydoobydoo on August 06, 2013, 04:56 am
Ron Paul has been accused by several others of selling bad information.

I don't have any personal experience but I would be quite skeptical buying anything from him after what I've seen on these forums.

Is this seriously the full text of what he sells?

Pathetic.
Title: Re: RON PAUL SYNTHESIS FAILURE (Anhydride for fun and profit)
Post by: funeightyone on August 06, 2013, 03:20 pm
Yeah, I fell for that same trick. Wasted $3500. RP pretty much crippled my game entirely. Still recovering from that loss. (going on 6 months) The man should really be banned as a vendor.
Title: Re: RON PAUL SYNTHESIS FAILURE (Anhydride for fun and profit)
Post by: DrDeepWood on August 09, 2013, 08:49 am
just because you failed at a synthesis does not make it a scam or a trick.
I have lifetime consulting for my clients for a reason.
But since you decided to post my guide open like that you are no longer welcome to buy any of my products and you are blacklisted from my free consulting services.
Title: Re: RON PAUL SYNTHESIS FAILURE (Anhydride for fun and profit)
Post by: Candy on August 10, 2013, 11:33 am
just because you failed at a synthesis does not make it a scam or a trick.
I have lifetime consulting for my clients for a reason.
But since you decided to post my guide open like that you are no longer welcome to buy any of my products and you are blacklisted from my free consulting services.

If you are still claiming that your guides are correct, I think that you should defend some of the issues being raised in the last couple of posts here:   

http://dkn255hz262ypmii.onion/index.php?topic=45417.msg1351579#msg1351579

Title: Re: RON PAUL SYNTHESIS FAILURE (Anhydride for fun and profit)
Post by: lokiju on August 13, 2013, 05:59 am
A guy once said that you'd never lose any money underestimating the intelligence of the US public (paraphrased). Acetic anhydride is useful stuff and  has been 'watched' for years. People in sciencemadness.org have come up with a synth for a small amount in a section of their site named 'prepublication'. Just don't post a question asking about obvious drug precursors, they get these questions all the time and will either ignore you or call you names because drug cooks have totally screwed up chemistry for ametuer chemists.
A guy named Lenoid Lerner has also published a book named 'small scall synthesis of laboratory reageants with reaction modeling' It's on Amazon.com and it's between a $125-150 book. It spells out in detail how to make thionyl chloride from SCl2 (both nasty chemicals causing severe burns but fairly easy to make) you'll need a laboratory glass kit, 24/40 size you can get Chinese glass pretty cheaply from ebay (Laboy) You can check out the book a little by Amazon ('look inside') and also Google (and you can go to other computers so that you can exceed their reading limit)
After you get your thionyl chloride and acetic acid (glacial) mix up the two and you'll get acetic anhydride. I believe that this is probably the easist synthesis, but I'm no chemist.
Keep in mind that there are a lot of people in state and federal pens who have attempted or have started to make an attempt to make a controlled substance. Just one action (buying a beaker for instance) and maybe some drug literature (like from Uncle Festor, or Strike or Shulgin's TIKAL and PIKAL) is enough to get approximately a 8-10 year sentence. If you lie to a federal agent that's a 10 year sentence (maybe they'll drop some charges when you do a plea deal, most cases don't go to trial)
If you're a 'cook' the DEA will offer just about any reward to anybody to bust you and get the publicity. Someone could murder somebody and if they know a cook, they can get a get out of jail pass (this happened in a case in Kansas where one chemist killed a guy with drugs and  then turned in his partner) It's good reading, the lab was set up in an abandoned missile silo, and they had some helluva parties there. It's easy enough to google to find the story, a local newspaper in Kansas had about a 3 part story on it.
Another interesting story of a drug cook's experience is on Rhodium CLEARNET WARNING http://www.lycaeum.org/leda/docs/3727.shtml CLEARNET WARNING. it's near the bottom, and perhaps some of the other stories,synths will interest you.
With all the publicity of NSA giving data to DEA which then distributes the data to local police (if not 'interesting' enough for the Feds) it would be crazy to do anything towards synthing controlled substances. They even tell the police to make up stories (parallel stories they call it) of how they got the initial info. \
The NSA scans every email in the world, or at least the main trunks of the internet. The US takes pictures, front and back of EVERY SINGLE piece of mail in the US. This we know, and we know that there is lot's more.
Spend a 'lousy' year in a county jail, it'll change your perspective towards fantasies like it seems you might have
It's dangerous enough just ordering through SR (you have disabled javascript in Firefox in the Tor Browser Bundle, correct?) Maybe another few years the 'environment' will be more friendly, thanks to maybe the US not being able to afford locking up 3% of their citizens. Don't win a 'Darwin Award' by doing something like attempting a synth that will effectively remove you from the gene pool.
You are not likely to get accurate advice over a forum of this type (Silk Road). People who point you towards 'citations' (actual experiments by chemists) would be the most helpful. 'Total Synthesis' by Strike, and 'Uncle Festers SOMM' series may be helpful, although I've heard that Fester is about 30% BS.
Of course, JMHO.
Title: Re: RON PAUL SYNTHESIS FAILURE (Anhydride for fun and profit)
Post by: hoobydoobydoo on August 13, 2013, 06:33 am
buying a beaker for instance and maybe some drug literature (like from Uncle Festor, or Strike or Shulgin's TIKAL and PIKAL) is enough to get approximately a 8-10 year sentence.

Ummm no.  You don't go to jail for buying a beaker.

This has to be one of the dumbest claims I've seen on here in a few months.
Title: Re: RON PAUL SYNTHESIS FAILURE (Anhydride for fun and profit)
Post by: Quazee on August 13, 2013, 06:51 am
Ron paul I knew you were a fucking joke, but really?
Sodium bisulphate is not ph up. It is a ph reducer. lol wtf really The dude most likely went and bought ph up from his pool store and fucked up on the 1st step.
Title: Re: RON PAUL SYNTHESIS FAILURE (Anhydride for fun and profit)
Post by: fractalglobal on August 13, 2013, 01:08 pm
Firstly, I hate to say I told you so...
Actually, that was a lie.  I love saying it.


After spending some money, taking some useless risks and failing miserably. I believe it is time to get some real conversations going on.

I wish this place could become more technical oriented. If someone has some real background and can teach me how to cook. Contact me. I am no time waster and i have money. You must be willing to accomodate to some conditions so dont waste your time trying to make a quick buck of me.


-if you have some chemistry background please do comment.
-Please dont post irrelevant stuff like " all the kids are gonna be baking at home" they wont....this not shake and bake stuff.
I fell for that marketing pitch, and this is way more complex than that.

Please do comment,
Regards.
Yeababy
Many of us that have both practical and theoretical experience in chem have said that we are more than willing to give advice for free.  Funnily enough, its those same people that were most vocal in calling out DDW.
Quote
Acetic Ahydride Synthesis:
You need sodium bisulfate, make sure its SULFATE not sulfide, it is used as an Acid ph up in pools.
An acid ph up? I've always wanted one of those!  Unfortunately, the laws of physics have held me back from acquiring one :(. 
Quote
Pour a 1/4" layer on a large pyrex and put it in an electric oven as close as possible to the heating elements.
I thought this was a guide for people who don't know chemistry, not for people who don't know how to use a set of scales.
Quote
Put the oven on broil and watch the powder.
It will start to melt and bubble, when it stops bubbling you are finished dehydrating it.
Another sign that its done is a white film will form ontop.
Let it sit in the oven until its cool, shit is dangerous molten hot!
Or, as an alternative to the entire first paragraph of this guide, stick it in the microwave for 5 minutes.
Quote
Now break it up, put it into a bag and smash it to tiny peices.
Load this in your blender and get it a superfine powder.
Its a little pungent, dont breath it in.
Now add an equal part of calcium acetate and blend.
Load this into a flask with a distillation setup, acetic anhydride will distill over as the two powders react.
If the reaction slows down because the two powders cake in,
very carefully add water to about 10ml of acetic anhydride to turn it to acetic acid, then pour this into the powders, will help wet it.
Once all your anhydride is distilled over good luck cleaning the glassware out, that powder cakes in there like crazy,
best best is do consider it disposable and do big batches to make it worth your time.
Fuck yeah, nothing makes me happy quite like throwing out expensive borosilicate lab glass. For those that prefer a synthesis that doesn't cost more than just buying the end product, piranha solution and a bit of elbow grease will clean the cake.
Quote


Propanoic Anhydride Synthesis:
This synthesis is very much the same except you use calcium propanoate instead of calcium acetate.
For this reaction you do not need to "wet" it, just mix the two powders and distill off!


Acetylation parameters:


Usually during acetylation you just have your substrate, what you are acetylating, the anhydride and a solvent.
For a much faster reaction you can use sodium acetate as a catalyst.
This is the compound thats present in those re-usable heating pads, with the little metal disk you click to start the reaction.
This is also safe to ingest so you dont always have to worry about cleaning it out of your product. I would use 2% compared to your anhydride.
So 20g of anhydride and .4g sodium acetate.
For anhydride ratio to substrate you can use anywhere from 10x to 100x molar excess,
I read a paper saying that there is no real hard and fast rule.
Nice to see you have some practical experience with acetylation, or at least, are capable of reading shit written by people who do, and then selling said knowledge for rather insane amounts of money.
Quote

di-proponyl morphine aka super heroin:

For this you need to buy morphine tabs, preferably instant release but im sure extended release will work too.
Wrong, the wax matrix will fuck any reaction attempted with the XR tablets unless they are properly extracted.  2 minutes of googling gives many examples of this.
Fuck going through the rest of this trash. Given the amount this sells for, you would expect DDW to at least read over it and fix the glaringly obvious mistakes. 


Hey, here's a(pretty useless) present for you OP, Jon's MDMA synthesis, re-written by DDW and subsequently sold on SR for roughly $700.  Admins, I understand that this has been posted before, and was taken down by a mod, if you do this again, I will just re-write it myself and post it in a new thread.  Plagurism is either allowed, or its not.  You cannot have a rule that one person is allowed to copy and then sell a piece of text, but another person is not allowed to copy, and then give it away for free.
Title: Re: RON PAUL SYNTHESIS FAILURE (Anhydride for fun and profit)
Post by: fractalglobal on August 13, 2013, 01:10 pm


Quote
This reaction is the golden goose, chemists have been hacking away at this forever. You must remember that many of the ratios, concentrations, etc are finely tuned, changing them will drastically change the reaction, which is not always the case. Do not alter the reactions or you will be pulling your hair out.
 
 
Safrole: This reaction actually will work with impure oil, some impurities such as eugenol will increase yields by lowering side reactions, this is not true for most reaction tho, just this one. You can use pretty crude oil, no need to distill. Just throw into a sep funnel and wash with an equal ammount of water then wash with an equal amount of ethanol. This should be clean enough to work, just make sure to adjust the amounts if you know the oil still has impurities. Also, certain highly reccomended US vendors have oil which phenolic impurities. These impurities actually help SN reactions and will interestingly enough INCREASE yields as opposed to hurt them.
 
Setup: For many of these reactions harsh smells/vapors will be produced, the best thing you can do is set up your water aspirator with a hose going down the sink, the surround the hose with a wet rag to prevent any smells from seeping up. Even if the reaction requires normal pressures, its good to run the aspirator on it with an inlet for air, so it doesn't pull a vaccum. This will suck any vapors into the sink water and straight down the drain.
 
Bromosafrole formation:
 
Add 190ml of GAA to a flask, then add 75g HBr. The amount of HBr will need to be adjusted because hydrobromic acid is not sold as 100%, usually its sold as 48% constant boiling solution, so a little more than double the amount. Cap the flask with a plug that has 2 holes, one of them leading to your vacuum aspirator, the other you will leave open. Turn on your vac aspirator. slowely add your acid (180g h2so4 100%, it wont be 100%, recalculate for your purity) with a syringe/burret to the solution, there will be foaming and fuming so do it slow. Once all the acid is added get the temperature back to 20C or less and add your safrole/sassafras oil (160g). Give it a few quick swirls then remove it from your aspirator and place in the freezer at around 0C for 24 hours. Don't stir this too hard as you will lose yield, just enough to mix then let it sit. Also don't let it freeze, up to 10C is fine if you don't have a freezer thats in range without being too cold.
 
Pour off the solution from the freezer into flask A, you are seperating the salts that have precipitated, do this slow and carefully. Do not mix, your compound will get stuck in the salts! Set aside flask A and add water to the solid materials until they are dissolved, then pour this into your seperatory funnel, extracting with either DCM or TCE once, then dumping the aqueous solution. Save the organic (DCM/TCE) layer aside in beaker 2.
 
Pour flask A carefully into a seperatory funnel also add beaker 2 contents, then add 2x its volume as cold water. A lower layer will form with your product in it (using dcm, tce will be upper possibly). Seperate off this lower product layer into sealed flask B.
 
Clean your sep funnel and pour flask B containg your bromosafrole and organic solvent. Add 1x its volume as water and then *slowly* add baking soda while stirring with a rod (no shaking here!), keep doing this until it stops fizzing. Once the solution is free of acid seperate the organic layer and throw away the aqueous layer. Put the organic layer back into the funnel and wash it with 1x volume of pure water, then seperate and remove the water. Do this again but wash it with saturated kosher salt water (no halides in the salt, look at the label). Seperate the organics and throw away the water.
 
The organics need to be removed so you are left with bromosafrole. You can do this by putting in a flask and adding a plug that only has 1 hole with a hose pushed through it, this hose is attached to your aspirator which is run with your water cold and full blast. This will distill off the solvent at room temperature, if you are using something other then DCM or TCE you may need a warm water bath under this flask.
 
Once this solvent is distilled you have a pure solution of bromosafrole. This must then be converted to iodosafrole in the next step, the Finkelstein swap. Most chemists think that you can use this bromosafrole directly and this is why nobody has really capitalized on this reaction. You must go through the next step and convert it to iodosafrole, this is very important for this method. Even though it is an extra step iodine is a much better leaving group and makes a much cleaner end reaction at standard presssure. If you skip the next step you must do it in a sealed container which is a bitch.
 
Do not let bromosafrole sit around at room temperature in an open flask. It is stable but it is also volitile so make sure to keep it in a small container and capped.
 
 
 
 
Iodosafrole - Finkelstein rxn
 
 
For every 20g of bromosafrole reacted in the next step, use 200ml of acetone and 13g NaI. Add the acetone and NaI then pour in bromosafrole and let this react at RT with slight manual stirring for ~30 minutes, wont hurt to let it run a little longer. The reaction will end very similar to the first one and will be "worked up" the same by seperating salts, adding 2x water and extracting, extracting the salts, combining extractions, wash (no baking soda needed, just water and brine washes) and then evaporating the organics to get your pure iodosafrole.
 
So now you have your pure iodosafrole ready to go, time for the next step.
 
 
Your crude methylamine.hcl should be prepared by reacting formaldehyde with ammonium chloride.
There is a photowriteup here:
http://www.erowid.org/archive/rhodium/clandestine/methylamine/index.html
 
There are some things to improve the process. Do it in a container which you can remove the crude MeAm.hcl from after the process. Instead of using a hotplate/etc what you need to do is get a large container that will fit your flask, add enough water to come up to the liquid level in the flask, not above it. Boil this water in the bath and keeping adding table salt to the bath until the solution is super saturated and does not hold any more. This solution will now boil around 105C constantly as long as the water level is kept steady. During the process you need to hook up your flask to your water aspirator, turn the water on low so that during the process there is a very low amount of bubbling, like carbonation rising. Not bubbling hard, just a little tiny bit. Follow these steps and you will have some very pure crude MeAm.hcl for the next step. Once the reaction has run its course
 
 
Last Step:
 
For this reaction you will be freebasing methylamine.hcl to release methylamine gas into isopropyl alcohol. You are going for a 20%+ concentration by weight of methylamine gas in dry IPA, higher concentrations will mean a better rxn. The methylamine must be present in 10-15x molar ratios, 10 being the bare minimum. For 200g iodosafrole you will need around 300g methylamine gas dissolved in 1500ml of dry IPA. So I would start with freebasing around 400g crude MeAm.Hcl from earlier to be safe. This will require about 300g of sodium hydroxide dissolved in minimal water to freebase it. You should add around 100ml of water to a stainless steel pot and then add your sodium hydroxide, this will get pretty hot, use the heat and keep adding water until most of the NaOH dissolves. You need to heat the water to get more than possible sodium hydroxide dissolved in it for the next step. If you use the bare minimal amount of water then you do not have to dry your meam gas, which logistically helps a lot. You then load this into a syringe and add it to your crude methylamine.hcl to create methylamine freebase, a gas, which is then bubbled into dry IPA. You should weight the IPA container before adding the gas, and then weight it afterwards to determine how much was absorbed.
 
 
Once you have your crude methylamine, scoop the correct amount into a flask to make a meam gas generator and install the 2 hole stopper. In one hole you will have a large 50ml syringe for adding your base solution, in the other a hose with a basic suckback trap, don't bother trying to dry the gas like many do, it will only cause problems and pressure buildups. I would use plastic tubing which is thinner than .25", the thinner the better. At the end of the tube place a loose ball of glass wool to make a disperser which wont cause a lot of back pressure. Between the end of the tube and the reactor you need a suckback trap. This is made by making another 2 hole stopper and placing it in a tiny flask. When the temperature of a reaction that produces gas changes there is a rapid suckback effect, this will happen once your reactor ceases to produce the gas and it cools down a bit, if you do not add a trap you could lose product. Place the tube straight into the IPA flask.
 
Cool the IPA in the IPA flask in freezer on the lowest setting then add a 3 hole stopper. 1 hole the gas tube from the suckback is inserted through, the other hole goes to the vacuum aspirator and the last hole is kept open. Its very important to leave this hole open, you can loosely stuff a wet paper towel in to prevent smell from coming out, but it needs to be open for safety, this reaction is run under negative pressure anyway so fumes wont pour out of the hole. Turn on your water aspirator on the lowest setting, just enough to clear fumes from the rxn. Use the syringe and suck up the first part of your super saturated naoh solution in the syringe and drop it into the crude methylamine slowly, at a rate which you can not smell the methylamine coming through the hole in the 3 stoppered flask. Once the correct amount of methylamine gas has been added by weight remove the 3 hole stopper and quickly add your iodosafrole, then insert a stopper with no holes. Its a good idea to tape the stopper onto the neck of the flask. Shake this around with a gloved hand, you should see a very rapid color change. Let this sit in the ice bath for 30 minutes to make sure it has totally reacted, then under good ventillation and being careful, slowly release the pressure on the flask and remove the stopper, add a 1 hole stopper and a tube going to your aspirator. Place the flask into a room temperature water bath and let the water aspirator distill off the methylamine and some alcohol. You know when its done when it no longer smells like rotten pussy fish. Pour this solution into your seperatory funnel and add an excess of 10% base solution. Once your base has been added a nice yellow/golden oil will fall to the bottom, seperate this and extract the rest of the solution with toluene/xylene, around 100ml per 10g expected yield and add this xylene/freebase to your golden oil. You can then either titrate the freebase solution with HCl solution or gas it in the standard way. There are two options depending on your situation. Titrating requires a distillation setup but it works better on the large scale, wetness of the solution is not as big a problem. Gassing is less materials intensive with simple equipment but requires drying and works better on the XXg and XXXg scale.
 
Titrate: To titrate the solution place your xylene/freebase solution in a flask. Use 15% HCl and add it dropwise until the ph goes from 10+ to around 6. Once you added enough acid then distill off solution until the flask does not look wet. As you distill off xylene water goes with it as an azetrope, toluene works better in this regard. You keep distilling the solvent until it looks like all the water is gone, this will be very obvious if you pay attention to the sides of the flask and the condensation, wet looking effect wet solutions have. At this point cap your flask and put it in the freezer, crystals will form inside of the flask, drain off the xylene. Titration tends to be dirtier than gassing so you may need to recrystalize.
 
Gassing:
A cup of epsom salts is microwaved while grinding every few minutes until it all looks dry and white, no longer clear. This is dehydrated epsom salts, very hydroscopic and can not be stored, must be made day-of. It is hammered to powder it a little. A few rocks are placed into a large plastic funnel to provide a flat base and then a filter paper is placed over it. The warm dry epsom salts are poured into the funnel providing a layer atleast 1.5 inches thick. This is placed into a small hole in a bucket, which is placed so that the seperatory funnel drips directly onto the filter and into a dry bucket. Once this xylene has been filtered it will be a very clear orange solution, ready for gassing. If its cloudy dry again or else you will slay your yield, so drip dry it slowely the first time. MAKE SURE IT IS CLEAR OR DRY AGAIN. Once you have this clear solution in a bucket set up a HCL gas generator
This is done by placing about 1kg damprid in a flask with a stopper which has a hole for tubing. Add 20ml of muratic acid at a time to the flask and quickly replace the stopper. As liquid hcl hits dry hcl gas will flow, pipe this into your DRY xylene/freebase solution and mda.hcl will precipiate, keep filtering whenever you are between gas flows from HCl addition. If you want you can skip filtering until the end but this way its easy to tell when the reaction is over, no more crops of crystals will appear.
 
 
Cleanup: Not usually needed unless you want to grow huge, clean, clear rocks or used the titration method
 
This method is called a dual solvent recrystalization, this has been done if your molly is a fine sand, not fluffy powder or small crystals:
First you need a large stainless steel pot, in this pot put your molly. Add either pure methanol or 99% IPA slowly until it is all dissolved. If you go overboard and add too much alcohol then you will just need more acetone later and it becomes wastefull, so add it maybe 20mls at a time. IF you have good ventilation and want to use less materials then you can let the alcohol boil while it dissolves the molly, you can use like 25% of the alcohol this way. Anyway depnding on your purity and alcohol temperature you should have around 1L to 3Ls of yellow/organge/brown molly alcohol solution.
 
Now you need some acetone, use 4x the amount of acetone as you have molly alcohol solution. To answer your questions there is really no difference between hardware store acetone which has been dried and reagent grade acetone. Actually ordering a large amount of high quality acetone is one of the more suspisious things you can do when it comes to chemicals suprisingly. You can dry the acetone by adding about a cup of calcium chloride (DampRid) from the hardware store per gallon of acetone. Let this sit for a day and pour off the acetone leaving the solids at the bottom. You dont want to use mgso4 with acetone, there may be minor reactions that go on. Anyway its a good idea to dry the acetone but not necessary for fresh hardware store acetone which has been stored correctly.
 
So what you do is have a jug of the acetone with a stirring rod, stir the acetone and add the alcohol solution to it, you can do it all at once then stir but its better to do it slow and i will explain why. The reason this method is so good is because when you acetone boil the molly there are still impurities in the crystal structure, dissolving in this way allows those impurities to go into solution, dripping the alcohol molly into acetone causes the crystal to reform, but this time as very fine poweder with acetone all around it. the slower you do it the cleaner it will be, but it can be done all at once. Once this is done cover, seal the container airtight and put it in the freezer, it must be air tight or moisture will leak in and lower your yields. When the liquid is ice cold you should recover your molly by clamping an old tshirt over a bucket, and filtering it. Then you can just put on gloves and twist the tshirt molly package around to compress it and let the juice out. Another way would be to get an apple juice carboy, drill a hole, add a hose barb and attach that to a water aspirator on your sink, then you can put a large buchner funnel on top and have a vacuum remove the liquid/dry it out. But the tshirt method and then spreading it in a thin layer is good enough.
 
 
 
Growing Moonrocks:
 
for 10g mdma use 250ml acetone, place the mdma in the acetone, it will not dissolve. carefully heat the acetone to almost boiling (dangerous fumes) and slowly stir and add water dropwise SLOW. When all the mda dissolves in the solution very slowly cool it. The slower the sexier the moonrocks.
Title: Re: RON PAUL SYNTHESIS FAILURE (Anhydride for fun and profit)
Post by: lokiju on August 14, 2013, 12:42 am
If you make any physical step (like buying a beaker) and they can prove that you had the intent to manufacture a contrilled substance, that is all that is needed for a manufacturing charge. Intent can be ascertained in many ways, by an informant (dude told me he was going to make MDMA) drug literature (secrets of methamphetamine manufacture, uncle festor) possession of other chemicals either required for the synth (also a seperate charge, possession of watched chemicals is a seperate charge)
In fact in Texas, a 3 neck flask is a felony in itself (possession).
So yes, in certain circumstances a beaker purchase can result (if other conditions are met) in long jail sentences.
More info can be learned from the old site the 'Hive'. I've heard different stories about the archive, that you can get it online (free) that you can a reduced version of the archive online, but there are at least some partial versions out there waiting to be downloaded, for free. Strike's books 'Total Synthesis II', and he's got another book out there ('Sources')to help source glass and chemicals. Secrets of methamphetamine manufacture version I, II, III, IV, and V are out there (free) (from Uncle Fester) too many others (well, I don't feel like trying to type them all out) to list.
Best thing is to take high school chemistry, a year of college chemistry and then organic chemistry (usually a 2 semester course) It's legal to own glass (although those purchasing it over ebay will be recorded forever, if you do so under your own name, and like the poster above says, it's better to use piranha to clean at the end of your experiments followed by acetone rinse. Piranha is sulfuric acid, concentrated with some hydrogen peroxide mixed it. Get it on a body part, you'll know it pretty quick, urgent care or emergency room know what chemical burns look like too.
Couple of other interesting books are 'complete book of escasty' CLEARNET WARNING http://www.erowid.org/archive/rhodium/chemistry/tcboe/index.html CLEARNET WARNING, a book by Jack B. Nimble "the construction and operation of clandestine drug laboratories'
I would think most likely somebody wanting acetic anyhydride is going to want to use it to turn codiene into much stronger semi-synthetic opiates, or of course morphine into heroin. Sciencmadness has a 30 page topic on this (acetic anhydride synthesis), the page (with pictures) that delineates the thionyl chloride/acetic acid process in here CLEARNET WARNING  http://www.sciencemadness.org/talk/viewthread.php?tid=9&page=21#pid149874  CLEARNET WARNING
Search the thread and see if you can find anything about 'sodium BISULFATE' or whetever was mentioned above. I don't recall reading of that 'facile' reaction.
If you are polite and phrase your questions in a scientific manner, you can 'feel' out various sciencemadness.org posters, but they (in general) HATE drug cooks. Maybe look up 'Turd' (his username) and peruse his threads, He MIGHT answer a question, and you might run into reactions that you are interested in. There are other 'phenylethylamine' oriented  chemists there, I leave it to you to decide who they might be. I'm not too optimistic about you getting instructions from them easily. Some situations can even introduce some illegality from too precise 'advice'
another link you might find interesting, there's a link for the 'entire' Hive forum (and other links) CLEARNET WARNING http://www.hipforums.com/newforums/showthread.php?t=430906&f=114    CLEARNET WARNING
imo, Silk Road forums aren't really the place to ask questions re: synthesis (JMHO)
Beware of too friendly people in this subject who are curious about 'where are you at'-just a suggestion.
These links above should keep you 'busy' for weeks/months.
I can't think of more hazardous 'hobbies' than synthesis of controlled substances, unless maybe 'energetics'. There's too many ways to kill yourself/get locked up. Unless youre 16, w/o a criminal record, you are unlikely to catch any 'breaks' in this day and age, and you're parents will probably go broke with attorney fees alone.
another CLEARNET ALERT http://www.bluelight.ru/vb/threads/449763-Cultural-Icon-Hobart-Huson-%28aka-Strike%29-Released CLEARNET ALERT. this link is about 'strike' aka Hobart Huson
Title: Re: RON PAUL SYNTHESIS FAILURE (Anhydride for fun and profit)
Post by: lokiju on August 14, 2013, 01:10 am
For those who believe that the first amendment doesn't have 'limits' (in addition to crimes like shouting 'Fire'! in a crowded theater), there is this CLEARNET WARNING LINK http://www.rcfp.org/browse-media-law-resources/news-media-law/news-media-and-law-spring-2003/authors-held-responsible-re      CLEARNET WARNING LINK

Apparently too much advice on a illegal subject can be illegal, I knew that there were some limits, but this is a little scary for future generations.

For  the poster above who  thinks it's ridiculous to believe that 'buying a beaker' can have you doing time (although I said they need other conditions too) If they bust you for manufacturing, they will go through you house and charge you for things like coffee filters, lye for drain cleaning, turkey basters, etc. Everything can have a 'dual' use, practically.
Truth really is stranger than fiction.
Title: Re: RON PAUL SYNTHESIS FAILURE (Anhydride for fun and profit)
Post by: lokiju on August 14, 2013, 01:15 am
You shouldn't have to pay any money for info re AA synthesis, and I'm incredulous that somebody is making money doing it (and it seems invalid info too)
Title: Re: RON PAUL SYNTHESIS FAILURE (Anhydride for fun and profit)
Post by: HCeline on August 14, 2013, 04:43 am
The synthesis that got sold to the poor op definitely is real it just doesn't seem that it is the way written.  here is a nice hive thread detailing some of the difficulties that ol ron forgot to mention http://about.mdma.ch/000462958.html