Silk Road forums
Discussion => Drug safety => Topic started by: paxpax on June 23, 2013, 03:50 am
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I have long been out of the game but have amassed a fair amount of experience in MDMA synthesis using standard non exotic routes. I have always been a fan of the small labs as, imo, produce the best and most cared for product. I'd like to share some of the experience with the SR crowd. If anyone has any questions on synthesizing MDMA or MDA or needs pointers on precursors acquisition or walk through on reactions ask away and I will do my best to answer.
As always, tips are appreciated but certainly not required.
1HMhfwAmAa846ig2R2ChVamzf8FRApBTVc
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Great man. We need more pure mdma in this world. It's magic.
I guess mdma from black pepper would be considered an exotic route?
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I'd love to know all about the synthesis of MDMA!!!
Firstly, what method do you have experience in? Shulgin I, II? Or Merk?
Also, which is easier to synth MDA or MDMA?
and lastly, precursor aquisition? Do tell, I've seen some on Safrole Oil on SR but wasn't 100% trusting of the vendor.
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Can you obtain precursors easier than having to take the oils from the trees?
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How much money would you say you need to put into the whole project of synthesizing?
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is that you ron?
I think Ron's synths were more on the exotic side. Not super exotic mind you, but certainly not middle of the road.
Optimum pH for an Al/Hg w/ MeNH2.HCl? Or, I guess, would you rather have extra NaOH or MeNH2.HCl floating around? For some reason the ol' Al/Hg just doesn't bring itself to reflux sometimes (using bonified 'tone :-\).
Also, I've heard differing opinions on gassing in DCM, compared to xylene. What's yours?
IMO MDMA is easier to synth than MDA. Unless you can get cyanoborohydride of course. But the ketone -> oxime -> MDA synth with an acidic Al/Hg did help make MDA possible for the closet chemist.
And the sass oil coming into the US is popped big time. Joy has barely had any orders in the past month or so and now the listings down so.... ::). Not saying I wouldn't mind seeing a vendor pop up *hint* ;D.
And please, no one discuss sources for precursor acquisition as it feeds the piggies.
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Well some of Rons may have been on the "exotic" side the one I saw had quite a few glaring errors in it. Here you guys go for your viewing pleasure his "bromosafrole route" and by his I mean he copied the work jon and others have posted for free, sadly he copied it wrong.
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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.
And shit for tips 1FU89Zi68iwd5WDGU83iLncdtjjbNyEMNj I will point out the errors for everyone
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IMO MDMA is easier to synth than MDA. Unless you can get cyanoborohydride of course. But the ketone -> oxime -> MDA synth with an acidic Al/Hg did help make MDA possible for the closet chemist.
Uhm what are you talking about? First off cyanoborohydride? do you mean sodium cyanoborohydride https://en.wikipedia.org/wiki/Sodium_cyanoborohydride ? Well that actually is a ton better at reducing things to secondary amines than primary amines, or basically its better at making mdma. My source is good old rhodium archives: https://www.erowid.org/archive/rhodium/chemistry/mda.nabh3cn.html Its actually the first sentence.
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Uhm what are you talking about? First off cyanoborohydride? do you mean sodium cyanoborohydride https://en.wikipedia.org/wiki/Sodium_cyanoborohydride ? Well that actually is a ton better at reducing things to secondary amines than primary amines, or basically its better at making mdma. My source is good old rhodium archives: https://www.erowid.org/archive/rhodium/chemistry/mda.nabh3cn.html Its actually the first sentence.
I'm just going to assume that you're joking and being coy here ;).
Of course I mean sodium cyanoborohydride. Any other cyanoborohydride's out there typically used in this application? It's also funny that you reference an MDA synth to prove your point. If you had sodium cyanoborohydride why would you use it to reduce PMK to MDMA when there are other suitable reducers more readily available (i.e. Al/Hg or NaBH4)?
G'day. 8)
p.s. Thanks for posting that synth too! I've been wanting to take a look at it (and pick it apart, of course ;D).
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Uhm what are you talking about? First off cyanoborohydride? do you mean sodium cyanoborohydride https://en.wikipedia.org/wiki/Sodium_cyanoborohydride ? Well that actually is a ton better at reducing things to secondary amines than primary amines, or basically its better at making mdma. My source is good old rhodium archives: https://www.erowid.org/archive/rhodium/chemistry/mda.nabh3cn.html Its actually the first sentence.
I'm just going to assume that you're joking and being coy here ;).
Of course I mean sodium cyanoborohydride. Any other cyanoborohydride's out there typically used in this application? It's also funny that you reference an MDA synth to prove your point. If you had sodium cyanoborohydride why would you use it to reduce PMK to MDMA when there are other suitable reducers more readily available (i.e. Al/Hg or NaBH4)?
G'day. 8)
p.s. Thanks for posting that synth too! I've been wanting to take a look at it (and pick it apart, of course ;D).
I don't actually know of any other cyanoborohydrides. I know that other borohydrides work in that situation really well. isn't PMK phenol methyl ketone? or acetophenone https://en.wikipedia.org/wiki/Acetophenone? reducing does not at least to my understanding of chemistry yield mdma. Yeah there are plenty of other reducers, sodium cyanoborohydride is just a better choice for this reaction at least then the two you proposed. While Al/Hg is the old school standard and works well, it is pretty damn toxic, and hard to dispose of while still respecting the environment in a clandestine setting.
No worries that has lots and lots of errors in an already super hard to pull off method. You can find the correct procedure online for free.
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If you mean using NaBH4 to make MDA I hear it gives lousy yields.
I guess youngsters nowadays must not read enough. PMK is piperonylmethylketone, or just ketone, or 'tone. Google doesn't bite.
NaBH4 would be the best choice for PMK -> MDMA IMO. Much better availability than it cyano sibling and it still gives 90% molar yields. Al/Hg's aren't that big of a deal to dispose of. Mother Nature is more pissed at Haliburton and those fuck-face huge companies dumping TONS of waste every day. Dumping out a gram or two of elemental Hg every weekend ain't too bad.
No need to quote wiki for everything, if I don't know what something is I'll look it up then ask around if I can't figure it out.
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when I said other borohydrides I was thinking of triacetoxyborohydride.
NaBH4 is the old school go to for making mda and actually does give some decent yields ala eleusis http://www.drugs-forum.com/chemistry/chemistry/eleusis/mda.htmland if used in the route you yourself said the closet chemist should take in your first post instead of the hg/cl2 you suggest http://designer-drug.com/pte/12.162.180.114/dcd/chemistry/mdaoxime.html you get a juicy 90%.
I might be a youngster compared to some, but before you claim I don't read post some correct information. Sorry when you google pmk you don't get an outdated non nomenclature name for mdp-2-p.
There is a reason I keep posting links to sources instead of just claiming things. I do it because you keep posting false information. I was hoping that by showing you how you were wrong you might be able to learn something.
Dumping mercury salts into the environment is not something my personal soul wants to be responsible for. Yes I agree with you its less harm than Haliburton's evil ass but that karma is on them.
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Please don't say I post false information as I've only voiced opinions. Many ways to do things and some work better for others, so some difference of opinion is to be expected.
Your eleusis link doesn't use NaBH4... so is it suitable for MDA production? Find the links!
If you can get di-isopropyl azido-carboxylate, hydrazoic acid, and triphenylphosphine then you are light years ahead of me and don't need anything at all. For Sonson's reduction well... go get some sodium and you're in business ;D! I think an acidic Al/Hg (what is a hg/cl ???) ala antibody would be easier and gives good yields, certainly better than eleusis' 65% yield, if it works, doesn't seem like he tried it, only proposed it. But yeah, the oxime route is the way to go. Need a link for that acidic Al/Hg :P?
Someone help me out here, this guy's crazy with the rare reagents. He's got benzene comin' out his blowhole!
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I'm saying you post false information because you make claims that are wrong and don't post any sources to back up what you say, but then again since the majority of what you say is WRONG your not going to be able to find sources to support you.
whoops wrong link that's what happens when you spend 15 to 16 hours a day researching. Here are two resources that use it: https://www.erowid.org/archive/rhodium/chemistry/redamin.titanium.ammonia.html and http://www.sciencemadness.org/talk/viewthread.php?tid=7218.
hg/cl2 is the basic easy to start with point for a mercury aluminum amalgam reaction. And once again if you feel morally comfortable dumping mercury salts into the environment go ahead, I for one choose other routes when they are available to prevent doing just that. Plus unless the chemist is quite skilled you will leave stray traces of mercury in your product which is a no no to anyone who may care about the consumer.
uhm none of those three are watched at all. triphenylphosphine can be bought for cheap as shit around 10-12 a kilo. di-isopropyl azido-carboxylate or cas 2446-83-5 can also be bought easily if searched for. Oh and look so can hydrazoic acid or cas 7782-79-8 as it is commonly used as a buffer solution.
I have more than helped you out, quite trying to act like you know what is up and post some sources or I' just gonna have to make you keep looking like a jackass.
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cas #4676-39-5. Still kind of surprised you couldn't find that one, especially considering all the research you do. Must not be researching well. I searched 'pmk cas' and it turned up a couple relavent articles. Also, why all the cas #'s ????
Please point out my false information and I will provide sources where I have them. I think the only one that isn't a Rhodium link is 'NaBH4 gives lousy yields of MDA.' Labtop was wrong that NaBH4 would work well for MDA. Sunlight (maybe someone else too, can't remember) ran some tests and found this out. Don't have the reference on that one because it's a hive archive post :-\.
Go ahead and order all that stuff from Sigma or Fischer ;D. I never said it was watched, just tough to acquire. Of course you can get damn near anything from large companies, everyone knows that, but why isn't everyone just getting everything from them then?
hg/cl2 is not the basic easy way to start an aluminum mercury (or just Al/Hg for those in the know ;)) amalgam. HgCl2 is the chemical you're looking for pal. I think any mercury salt works though (hive ref.). Moral issues: Anyone who is making drugs a hundred grams at a time (small scale, but still a thousand hits) probably doesn't care about dumping .2-.5g of Hg (notice it's elemental mercury after the reaction is over). You haven't truly chosen any route until you've performed it ;D. I choose routes that are doable, sorry environment. I don't think it takes a skilled chemist to do an acid base work up. Pretty basic task really. Care for the consumer is paramount, it's why we do things like recrystallization.
You haven't helped me at all. To think you have is asinine. I understand that you just finished AP chemistry and mom won't let you do experiments after midnight so it's tough to try new (or old) things but please leave the chem up to more competent people. Posting shit like "unless the chemist is quite skilled you will leave traces of mercury...blah blah blah." is misinformation. Doing a proper work-up (i.e. acid base followed by recrystallization, kick a vacuum distillation in there for some serious purity) is PLENTY to get rid of any and all remnants of mercury. In fact, I'd be surprised if mercury has ever made it through to product.
Eagerly awaiting your reply... I'm sure it's the first thing you'll do when you get home from school since you don't have any real chemistry to do ;). Mom will be proud when you cook up your first gram(s) and the environment is still smiling.
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cas #4676-39-5 is mdp2p one of the most watched chemical precursors in the world. Sorry when I was trying to provide you with some clues to a doable route in present climate. Obviously your happy still existing in circa 1985 back when you just just get drums of the easy stuff. I gave you the cas# because suppliers that will sell to individuals pop up (try looking a little further down the results those companies need not be used for shit) when they are googled.
You still make claim's yet fail to provide proof that anything you say is correct. I have consistently backed up all claims I have made with links something you have yet even attempt. It really would have been easy to have a nice dialogue trading links back and forth, but nah you would rather just sit there and try and make up for your lack of any actual knowledge through petty insults.
here's a good searchable hive archive: post proof: http://chemistry.mdma.ch/hiveboard/index.html then feel free to talk all the shit you want.
here's some stuff about common impurities found in the clandestine labs, one of the most common forensic techniques is identity by levels of impurities that have been left in the product. I would be willing to bet that 99.999% of labs making mdx's that regardless of how well cleaned there will be impurities left. https://www.erowid.org/archive/rhodium/chemistry/mdma.redamin.impurities.html http://www.fsijournal.org/article/S0379-0738%2804%2900446-3/abstract hgcl2 is the starting point for antibodies and chromics versions of this method which are probably the most common not sure why you hating on that as you brought it up? Yes I will agree with you there would only be half a gram of mercury salt remaining, now the world health organization says the safe amount is 1.6 micrograms. You see the difference there? I'll also agree with you that it doesn't take a skilled chemist to do an acid/base workup, yet that doesn't even begin to come close to pharmaceutical grade standards. Shit you could do ten acid and base work ups and it wont remove all the impurities. not sure about this 100 percent of the time but in a clandestine lab the luxury of pharmaceutical grade quality control is just hard to find.
Alright I'm glad I haven't helped you out, you obviously know everything there is to know. I would hesitate before you stoop to insults tho as you still just keep talking out your ass, and I just keep quoting facts back at you. And when product is made through that route I doubt there has been a lot of times when mercury hasn't made it into the product. I would like to direct your attention to the forensic papers I already posted. The standard work up is essential, vacuum distilling your freebase is probably also essential, yet neither of these things will remove all impurity and lead to a pharmaceutical grade product.
It seems I have just a tad more respect for are earth than you, I'm not meaning that as an insult I just don't want it on my spirit. I'm gonna even keep trying to be nice to you: surprise green chemistry: http://about.mdma.ch/000432241.html http://about.mdma.ch/000432241.html. That wasn't that hard now was it? Oh wait you don't want my help or you already knew all that or something
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You say I'm incorrect but you're not pointing out where. Where am I incorrect?
clearnet links coming up.
NaBH4 to MDMA with good yields : http://www.erowid.org/archive/rhodium/chemistry/redamin.nabh4.html
thread about NaBH4 giving lousy yields on MDA : http://chemistry.mdma.ch/hiveboard/methods/000208935.html
oxime to MDA via acidic Al/Hg : http://www.erowid.org/archive/rhodium/chemistry/alhg.oxime.html
MDA via the cyanoborohydride (sodium of course ::)) : http://www.erowid.org/archive/rhodium/chemistry/mda.nabh3cn.html Sporting a moderate yield but good for the scale up
Don't have any ref's for Hg not being in the product but your refs don't say either way. I think we're both being a little extreme on this issue (to prove our points no doubt). What would the pharmaceutical industry do passed an acid base, vacuum distillation, then recrystallization? Chromatography? The W.H.O. says the safe amount is 1.6 micrograms... in what? a liter? a body? mg/kg? Your ref's are pretty weak on this one. Anywho, with no refs on my side I still contend that elemental mercury is easy to separate from a reaction matrix.
If you want 'doable' in today's climate I'd suggest routes starting from non-safrole precursors. But that's another conversation.
Oh, and I never hated on the Al/Hg, just wanted to point out how you don't seem to know the nomenclature. This part is just opinion (you had a bunch of those with no ref's ???) but I feel like osmium and roundbottom's Al/Hg's are more common. In fact, chromic's is just roundbottoms. I'd give you the ref but instead I'll just let you make sure the ratios are identical, I'm sure you already have the molar ratios worked out in your notebook because you're so close to completing a synth.
Anyway, this is silly. Let me know where I need ref's and I will post them for you. If I'm wrong that's fine, another opportunity to learn. No offense (seriously none intended) but it doesn't seem like you practice chemistry. Maybe you do chem in a professional setting (i.e. real job in a lab) and aren't used to clandestine methods, I don't know, just doesn't seem like you practice. Seriously no offense intended, I know it's an offensive question is why I'm strongly saying I mean no disrespect.
In order to try to move this dialogue in an amicable fashion let me say this... What's your favorite route for making ketone? You probably have some juicy ones saved up. Peracid and benzoquinone routes have their ups and their downs, I just don't approve of the pressurized O2 wacker. No ref's on that one, personal experience. If you check the hive though it's full of mixed opinions on it. Some insist it works like a charm, others can't get it to work.
I do sincerely thank you for the searchable hive archive. Do you know what year(s) it covers?
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When going from Helional via Oxime to MDP2P, what is the contaminating ketone and how does one get rid of it?
If you can help me figure this out, I may shit my pants with joy and tip you big time.
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Lol your references back up my initial statement that set you off, that sodium cyanoborohydride is better at reducing things to secondary amines than primary ones.
The second reference from the dea actually has a nice little blurb in it about mercury contamination being an easy way to identify that route and how its easy to use to convict folks after the fact to amounts found over the course of an investigation. A pharmaceutical company would be using those steps, chromatography included, on every step of the process. On top of that there is heavy testing done to make sure each reagent is at the highest purity level in every step in the reaction. They have access to high end testing equipment none of us in the wild do. Here is a nice list of some operating procedure to just give you kinda of an example what goes into it http://www.pharmaguideline.com/2008/01/pharma-sops.html. The WHO number is an exposure amount so I guess it would probably be per kg? or per body?
uhm just because you start a statement with no offense does not magically make it non-offensive. That would be like you saying no homo and then slurping down a fat cock, but sorry bro that still makes you a rump wrangler. Believe whatever you want about me. From all your comments I doubt you have so much as cracked open a real chemistry book much less stepped into any form of lab, clandestine or other. Go back to jerking off to the rhodium archives bitch, and imaging how much of a bad ass you could have been twenty years ago. Actually news flash pull the dicks out your ears, your lack of knowledge and even unwillingness to be spoonfed, means you will kill yourself attempting this shit. Actually worst case scenario you don't kill your self but poison some innocent people with your firez drugzz. Better you just up with your bizarre masturbatory fantasy about being a leet drug cook, and leave the chemistry to the chemists.
Now that nastiness is behind us and your going to be amicable I might as well return that curtsey. The only method I've had personal experience was with buffered peracetic. then using hcl for the rearrangement from the glycol. Getting my hands on safrole to play around with has been incredibly difficult so I haven't invested alot of research into compiling these routes. Almost all my practical experience in the field of methylenedioxy chems has been starting with that lovely ocean smelling gem. At present moment I have been working on a way from vanillin here are my thoughts:
1. acid-catalyzed crossed aldol condensation between vanillin and MEK gives the expected a-methylphenylbutenone
2. oxidation with hypochlorite gives (as a methyl ketone) the a-methylcinnamic acid and chloroform.
3. Reduce this
4. followed by methylenation of the phenolic diol, would give a-methyl-3,4-methylenedioxyphenylpropionic acid
5. Form the amide from that
6. then a Hoffman reaction (hypochlorite again) directly to MDA.
I have no idea the date on that archive I'll ask the guy who gave me that link tho.
When going from Helional via Oxime to MDP2P, what is the contaminating ketone and how does one get rid of it?
If you can help me figure this out, I may shit my pants with joy and tip you big time.
You don't make mdp2p from helional via the oxime. look at the two structures of mdp2p and helional. look at the lengths of their carbon side chains. Now look at the positions of the double bonded oxygen. I believe you are confusing two routes. All of the ways I have seen with helional do not go through mdp-2-p.