Author Topic: OTC MDMA is now easy and cheap!!  (Read 32627 times)

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Agent_Smith

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OTC MDMA is now easy and cheap!!
« on: July 11, 2001, 12:55:00 AM »
Welcome back bees.  It's amazing what you can do when you put your mind to it...  with the Hive gone, I've been forced to do a little research of my own.  So I researched, I tested, and I smiled, because there now exists an easy OTC synth of MDA, MDMA, MMDA, etc. without using RP of I2.  Behold How I made my first sucess!  (I wrote this write up for a friend w/o any chem knowledge, so its a bit basic.)

Agent_Smith's Easy OTC MDA synth:

Heres how this is going to work.  First, the safrole is going to halogenated.  Then, it's going to react with ammonia in order aminatate it into the lovely amphetamine derivative.  Boom, MDA.

The halogenation

The halogen you're going to use is bromine.  Fluorine is much to reactive to be safe with.  Chlorine won't work because it won't "mix" well with the safrole, needs a surfacant.  Bromine is easy to come by, cheap, and more reactive than iodine.  Iodine would work, but iodine salts are watched chemicals, and OTC iodine is expensive.  Also, iodine will require red phosphorus, which... sucks. 

Now, since we dont want to brominate the ring, were gonna use HBr rather than Br2.  HBr is a bitch to make.  I'll discuss quickly the ways of making it so that you don't feel compelled to find an easier way that won't work. 

NaBr is easily available OTC.  You can make HBr by reacting NaBr + sulphuric acid -> HBr + NaHSO4.  The problem is that HBr reacts with sulfuric acid to make Br2 (more like a sick solution of Br2 and a bunch of crap, but the key peice is that it doesn't make HBr).  NaBr and phosphoric acid should work, however, it requires heating under pressure to do so, which is impractical (heating at atmospheric will boil away the water before any HBr is released). 

 Thus, to generate the HBr gas we need to brominate the safrole NOT on the ring, we're going to brominate another aromatic ON the ring.  (Head spinning, ain't it?)

Ok, so, in order to brominate something on the ring (thus releasing HBr), we need Br2, which will be made by tearing the bromine out of NaBr (sodium bromide).  This can be done the same way that bromine is extracted from seawater (where NaBr exists in low concentrations).  The reaction is Cl2 + NaBr -> Br2 + NaCl.  Thus, we're going to gas a NaBr solution with chlorine in order to release bromine and table salt.

Chlorine will be made from pool shock (calcium hypochlorite) and muriatic acid (HCl)  Here's the procedure:

Making Chlorine

1) Make a chlorine gas generator.  Goto the hardware store and get 6 feet of 1/4" Polyvinyl tubing.  It's the small clear stuff.  Cut it into a 1 foot section and a 5 foot section.  One hose is going to put HCl in, the other is to take Cl gas out.  Now, cement, tape, expoy, or otherwise seal the two tubes into the neck of thebottle.  They should only eneter the bottle about 1 inch.  Find a syringe, at a local pharmacy.  Not a hypo. needle mind you, but just a syringe.  They can also be gotten at hobby stores.  Fit the nipple of the syringe into the 1 foot section of hose (you may need to use a different size hose, or tape things up to get a good seal. 

2) Goto the hardware store and pick up some powdered pool shock.  On the front of the package you'll find it's ingredients.  You want the highest percentage of calcium hypoclorite that you can find.  78% is the best I've seen, in "Super Sock It".  While you're there goto the cleaner's section and grab a liter or so of "Muriatic acid."  Chlorine is extremely toxic, it'd be a good idea to get a gas mask (not just a painters mask) while you're there.

3)  Fill the beer bottle about 1.5 inches high with powdered shock.  (This will require unsealing the hose from the bottle unless youre very patient and want to add it through the hose).

4) Now, fill the syringe with muriatic acid (HCl).  When you squeeze the syringe, the HCl will hit the shock and chlorine will come out of the longer hose.  You've got enough shcok in the to make a bunch of chlorine.  You'll have to refil the syringe about 10 times or so to use all the shock.  Stir the bottle before you unhook the syringe to refill it to make sure it's done reacting.

Now, using your chlorine gas generator you're going to gas a NaBr solution to release the bromine therein.  Theres a problem though.  Bromine is soluble in water, just like NaBr.  A bunch of the bromine is going to be lost into the water.  Also, bromine is liquid at room temp, but it's volitile.  That means it's going to make oodles of fumes, poisonous ones, so wear the gas mask that you should have bought by now.  In the future, you can cut costs down a whole bunch by finding something that NaBr is soluble in, but bromine is not.  I'm looking into this now, I'll let you know if I find something.  Here's how you'll make your bromine:

NOTE:  Apparently dropping H2SO4 onto a solid mixture of MnO (the balck stuff in Duracells) and NaBr will make bromine with the problem of loss into the water.  I haven't tried it though, but I have a feeling that it will work MUCH MUCH MUCH better than this.

Isolating Bromine

1)  Get Spa Bromine Base or Spa Brominator from Ace or Home Depot (Home Depot has it cheaper).  Make sure the ONLY ingredient listed (besides a few % inerts) is NaBr or sodium bromide. 

2)  Dissolve 40g of the bromine in 200ml (200g) of water.  You can use more if you want more bromine (you'll need a bunch, you'll have to do this many times, I'd proably do a large batch), but keep the NaBr to water ratio the same or even lighter on the water if you can get the NaBr to dissolve.  Don't use tap water for anything, use distilled. 

3)  Put the NaBr solution into a beaker or pitcher with a pouring spout.  This is important that the container has a spout, you'll see why in a second.

4)  Take the long hose for your chlorine gas generator and put it into the NaBr solution, and lay the hose into the pouring indentation/spout. 

5)  Take a large glass bowl, and fill it with ice water, very cold.  Put the bowl on top of the NaBr beaker.  The fewer gaps you have, the better.  You don't want to lose bromine to the air, but don't seal the bowl on, because the chlorine still needs to escape.

6)  Start slowly squeezing the syringe to produce chlorine.  The solution that was clear will turn orange, then red.  It will still be transparent.  After several minutes of gassing, the solution will turn cloudy red instead of transparent red.  I'm not sure why, but it seems that you don't gain anymore bromine after that point.  Let all the cloudy shit settle.

7)  Using a pipet (or a syringe) suck the black liquid off the bottom of the beaker.  Avoid grabbing any water.  Store this in a glass bottle with a plastic cap.  Don't use a rubber stopper or cap.  Don't use metal.

Making a Catalyst

Ok, that was the hard part, it gets easier now.  Once you've got about 50mls (150g) of bromine, you're ready to go.  I'm not taking the time to calculate exactly how much you'll need, but that should be enough to get a good yield from about 30g safrole.  Remember that bromination of an aromatic ring normally requires a catalyst.  Thankfully, iron reacts with liquid bromine to make FeBr3, and ideal Lewis Acid catalyst.  Get some Ultra Fine steel wool..  Get the finest you can.  Tear off about a gram and throw it into your bromine.  It might bubble a bit, but it will be dissolved into the bromine.  Now you're ready to make HBr and brominate your safrole:

Brominating Safrole

1)  Empty your Cl2 gas generator and clean it out. 

2)  Pop the bromine/catalyst solution into the bottle.

3)  Get some old fashioned mothballs.  You'll notice that they are nearly 100% naphthalene: perfect, an ideal aromatic.  Crush about 100grams of mothballs, not too fine though, leave it chunky.  You're going to add this is two additions, so divide it in half.

4)  Take the long tube from the gas generator and put it into a bottle of 30gs of COLD safrole.  Run the tube through a cold water bath before it reaches the safrole, this will cut down on how much bromine is released (It's not really a prob. but bromine is a volitile liquid).  It'd be ideal to have a bromine trap chmaber, but it is optional.  The ~30gram bottles of sassfrass work great as a container to brominate in.  Plug up the short tube, you're not going to use it.

5)  Throw in one half of the crushed mothballs and quickly seal the gas generator.  When the reaction stops completely, add the rest of the mothballs and seal again.

NOTE:  This reaction might give higher yields if it is conducted with the safrole dissolved in about 200ml of chloroform.  You can make that by getting a bottle of liquid pool shock from Ace, and popping it into a bucket with a full bag of ice.  Then add a cup of acetone (Acetone, not nailpolish remover),  Wait 30 minutes, and you'll have about 100mls of chloroform as an oily clear liquid at the bottom of the bucket.  Do that twice.

You now have bromosafrole.

The Amination

Kudos to Iudekx, this procedure is nearly verbatim from his OTC MMDA synth.

All you have to do now is react it with ammonia.  You'll need ammonium sulphate fertilizer.  This can be hard to find but it's readily avaiable at hardcore farm supply stores.  This will be reacted with sodium hydroxide (red devil lye, or some kinda of crystal drain cleaner, not Crystal Drano) to release ammonia gas.  HEED MY WARNING AMMONIA WILL KILL YOU FASTER THAN YOU CAN SAY "OOPS, THAT SMELLS FUNNY."  A store bought gas mask won't protect you from ammonia, you'll need to buy different cartridges for the mask to be safe.  The store might have ammonia proof cartridges, I don't know.  Heres what you have to do:

Methanolic Ammonia

NOTE:  if you want MDMA, you can make methylamine (good synth on rhodium's site) and put it in the methanol instead of the ammonia.  Yields will be better, but you'll have to invest in researching that on your own.

1)  Go get a mason jar.  Ask if you don't know what that is.  Get a bottle of gas line treatment, yellow bottle blue letters too.  That is methanol.

2)  Put the methanol into the mason jar, along with the long tube from the gas generator.

3)  Pop 140g ammonium sulphate into the gas generator bottle.  Dissolve 80g of lye into a bunch of water, but be wary that it can fit into the gas generator.

4)  Setup up the generator like you did for chlorine, and use the syringe to add NaOh and bubble ammonia into the methanol.  When all the lye has been added (might need to do 2 runs), pour in the bromosafrole, and seal tightly, VERY TIGHTLY.

Shake the jar every now and then for 7 days.  The longer you let it cook, the better yield you'll have.  You can heat it to speed up the reaction, but that will pressurize the bottle and it may explode... your call if its worth it.

After 7 days, carefully open the bottle, wearing your ammonia proof gas mask.   Then, do this to recover your MDA:

Extraction

1)  Grab your syringe and your HCl.  Fill the syringe with HCl, and slowly! drip HCl dropwise into the jar.  When the drops hit the jar, it will make a cloudy solid, ammonium chloride.  Add HCl until pH 2 or so (get test strips from any chemistry set).

2)  Filter the solution, discard the solid, and put the liquid on a large flat glass pan.  Put this out in the sun and wait for the methanol to evaporate (wont take long, methanol goes quick). 

3)  When all the methanol is gone, you'll be left with a powder covering the surface of your dish.  Guess what that is?

NOTE: it'd be a good idea to do a standard A/B extraction, this way is pretty dirty, but it works.

That's all I know.  Agent_Smith out.


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Rhodium

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Re: OTC MDMA is now easy and cheap!!
« Reply #1 on: July 11, 2001, 01:05:00 AM »
This method works all fine and dandy in theory, but what kind of yields can be expected in real life? I see that your post is lacking much detail, so I wonder, have you tried it out in practice, and what was your yield in each and every step?


http://rhodium.lycaeum.org


Agent_Smith

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Re: OTC MDMA is now easy and cheap!!
« Reply #2 on: July 11, 2001, 01:14:00 AM »
Yes, I tried it but once.  I've run into some trouble with the law of late, so I've decided to retire for a while, and won't be trying again soon. 

The run I did was around 70% in the halogenation (in chloroform) and 50% with a 12 day amination (ammonia).  I think 50% is the upper limit on ammonia aminations, if you want higher yields I'd use methylamine.  Also, for the whole process, if using chloroform and methylamine, I wouldn't expect anything over 70% (start to finish), with 80-85% yeilds possible with methylamine amination (based on others experiences).  The longer you gas in the first step, the better yields...

Still worth it if you ask me, all the 'cursors are so cheap.  The hard part really is the HBr, but I swear to god it works perfectly.

The bromine from the NaBr is the slopiest part.  You'll get only a few grams of bromine from 40g NaBr with the chlorine gassing in water (I tried this in a FBF with a reflux condensor as well, yields were no better).  Another solvent needs to be found, perhpas one where bromine is insoluble.  If I did this again, I'd use the NaBr and MnO mix + H2SO4 method to get the bromine.  Refs for that are everywhere, I dont have the eq'n offhand.


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Rhodium

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Re: OTC MDMA is now easy and cheap!!
« Reply #3 on: July 11, 2001, 01:38:00 AM »
Acidify a concentrated NaBr (or KBr) solution with H2SO4, thereby getting aqueous HBr. Add H2O2 of any available concentration to oxidize the Hbr to Br2. You now have a dark red solution consisting of many things, but only the bromine is soluble in organic solvents like DCM, so just extract it from the aqueous phase.

It is a byzantine route to dry HBr you propose, but it is indeed creative.


http://rhodium.lycaeum.org


Agent_Smith

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Re: OTC MDMA is now easy and cheap!!
« Reply #4 on: July 11, 2001, 02:05:00 AM »
byzantine indeed, but can you propose a better one?  I've tried em all, this one works.

Thx for the Br2 info, i didn't know it was the only thing that'd be soluble in organics.


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Rhodium

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Re: OTC MDMA is now easy and cheap!!
« Reply #5 on: July 11, 2001, 02:14:00 AM »
I am not experienced with OTC routes, as I do not know exactly what is OTC in the US. There are better routes to MDA, but they will normally use at least one precursor or reagent that is not OTC.


https://www.rhodium.ws


Agent_Smith

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Re: OTC MDMA is now easy and cheap!!
« Reply #6 on: July 11, 2001, 02:22:00 AM »
Well, I thought it was worth posting for a few reasons, even though its not the best way to make MDA:

It is totally OTC, and probably OTC everywhere in the US

Unlike some other OTC routes, it doesn't require any tedious steps like stealing 80 bottles of I2 or scraping RP

The oxone method seems promising, but requires a bit of glassware, especially if the reduction is going to be done right.

So regardless, I consider it valuble, and for my situation, it was destined to be the perfect route.


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methadone

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Re: OTC MDMA is now easy and cheap!!
« Reply #7 on: July 11, 2001, 06:35:00 AM »
does the dmso method work?
Dmso+NaBr+oil==> bromosafrole???

Agent_Smith

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Re: OTC MDMA is now easy and cheap!!
« Reply #8 on: July 11, 2001, 06:59:00 AM »
Some (few) have said they made the DMSO route work, but it's my impression that the vast majority of people who try, fail.  Regardless, the DMSO rxn is indeed one thats highly sensitive to temp. and scale, and take a longs time. 

Thats another reason I feel this is valuable, it can be done on an afternoon, while the other methods (DMSO, oxone) require setups for many days.


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methadone

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Re: OTC MDMA is now easy and cheap!!
« Reply #9 on: July 12, 2001, 05:21:00 AM »
is there an easy way to make HBr gas from NaBr...and then just bubble that into glacial acetic acid ..like TS2 suggests..??

Agent_Smith

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Re: OTC MDMA is now easy and cheap!!
« Reply #10 on: July 12, 2001, 07:15:00 AM »
wtf do you think the whole procedure here is doing (see paragraph 5)?  And don't use acetic acid, use chloroform.  better yet.. just follow the procedure.


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AMINATOR

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Re: OTC MDMA is now easy and cheap!!
« Reply #11 on: July 12, 2001, 09:35:00 PM »
Yo! Agent smith! congrats to your Hbr method...you musta busted your ass cookin up that scheme, nice to see you...
anyway... here's a way to speed up your aminations and improve yields....

soak 40 bounce dryer sheets in a 32 oz. jar of methanol or isopropynol and shake well, for maybe 10 min. or leave overnight.
pour out the alcohol into a pyrexdish and ring out the bounce sheets then evaporate the alc. now scrape your quaternary ammonium sufactant from the pyrex evap dish while avoiding the scummy residue on the sides.
and voila!! your very own OTC quatenary ammonium phase transfer catalyst.  with this it might be possible to do a reasonable delepine reaction with hexamine or relativly kick ass reaction rates and yields for ammonia and definately kick ass yields for methylamine  8)  8)  8)  maybe someone can think of a way to purify the PTC....if its ammonium salts I guess you could probably just do an A/B extraction...also you could probably get your bromo compound with the PTC and HCl gas and finkelstein style bromo-swap or for that matter Iodo-safrole. you can get KI/NaI from photography stores, salt licks.

Here's also a little inspiration for a NaI synth, though it would be probaly be easier to buy from a photo shop:

Powdered aluminum(flash powder)
I2 crystals
H2O
sodium hydroxide

Mix the iodine and aluminum powder intimately (Mortar and pestle) and anhydrously!!(will start fire with a drop of water and release HI and vaporous I2)It will probaly make a little HI gas while mixing due to air humidity and moisture in the aluminum powder(maybe dry Al powder in oven?don't use tincture I2 unless it is thouroghly dryed!!)

Now, heres the trick...hydrolysing the aluminum iodide to form HI. I don't know if you could pour the mixture slowly into the h2o to form it or reflux the shit added separatley to the water...but any way, once you made the hydroiodic acid all one needs to do is react sodium hydroxide to form sodium iodide and evaporate the water.

I just thought of this idea for a little inspiration this is not a tryed or tested method of producing NaI, every one.

Is there anyway of producing sodium metal from the hydroxide or chloride etc..or an otc source or maybe potassium? these metals would react vigorously to create NaI/KI. don't know how dangerous it is though.... ok I'm outa here

BieneMaja

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Re: OTC MDMA is now easy and cheap!!
« Reply #12 on: July 13, 2001, 09:37:00 PM »

Is there anyway of producing sodium metal from the hydroxide or chloride etc..or an otc source or maybe potassium? these metals would react vigorously to create NaI/KI. don't know how dangerous it is though.... ok I'm outa here



electrolysis of an NaCl/KCl melt. but there are only a few bees who are able to go this way. alkali + halogene always react *ipmressive*. there are more usable ways available.



ea vita est via in caelum (seneca)
[this life is the way to heaven]

AMINATOR

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Re: OTC MDMA is now easy and cheap!!
« Reply #13 on: July 14, 2001, 12:03:00 PM »
I once heard of a "collision" reaction that involved gasing bromine with HI and it releases Hbr I wonder, if you made the aluminum Iodide and dropped small amounts in at a time in a solution of bromine and a hint of water, would it create Hbr gas? Maybe it would react slow enough to just dump it in?would this offer better yields of Hbr?
ahh maybe the aluminum would start to react with the bromine too....I don't know,just a thougt. hmmm.  ok how about this throw aluminum into slightly aqueous bromine and just let it make aluminum bromide that is hydrolysed by the water and makes Hbr in better yield. wudya think?...too exothermic? I wonder if the water would calm the reaction...

AMINATOR

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Re: OTC MDMA is now easy and cheap!!
« Reply #14 on: July 14, 2001, 09:34:00 PM »
Another thing that comes to mind, Agents Smith, is that if the sodium favors chlorine over bromine then why couldn't you drip hydrochloric acid on the NaBr to get your HBr. seams logical but I really don't know...I really like your sythesis idea and would only like to see it improve. I'd try this reaction myself but I'm flat broke right now. I appologise if it seams I am degrading your lovely procedure and all your hard work by suggesting different methods. I'm only trying to help.

Rhodium

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Re: OTC MDMA is now easy and cheap!!
« Reply #15 on: July 14, 2001, 09:55:00 PM »
Mixing hydrochoric acis with solid NaBr would create a solution, containing water, Na+, H+, Cl- and Br-. No HBr gas would be evolved, and certainly not anhydrous HBr gas, which is what we are looking for here.


https://www.rhodium.ws


Agent_Smith

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Re: OTC MDMA is now easy and cheap!!
« Reply #16 on: July 14, 2001, 11:16:00 PM »
No no, aminator, feel free to suggestions.  I know my synth is... "byzantine"... but for me it was still hugely economical. 

I have, however, struggled with the NaBr and HCl idea a few months ago.  It makes lovely plume of white gas, but alas its HCl, with a very small amount of HBr mixed in.  It'd be sweet if that'd work though...


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Osmium

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Re: OTC MDMA is now easy and cheap!!
« Reply #17 on: July 15, 2001, 01:10:00 AM »
I suggest you all get a little more practical experience and some theoretical background as well. I don't see much viable useful information posted here. Simply throwing a few tidbits you heard about or saw in a chemistry book together will not provide you with a working synthesis for anything.
And don't throw all kinds of different syntheses and precursor preparation ideas into one thread, it gets way too cluttered, confusing and unreadable and after some time nobody will answer the questions anymore.

Sure Al and I2 will produce AlI3, but only a beginner would be brave (and stupid!)enough to mix them dry!
Adding anhydrous AlI3 to water will hydrolyse it, but you still end up with an aqueous solution of Al(H2O)6?I3 and only very little gaseous HI.
And sorry, I won't even comment on the suggestion of reacting alkali metals with elemental I2...

Don't try to reinvent the wheel, there are working syntheses for all these compounds around already. UTFSE, and don't clutter one thread with all kinds of different ideas, at least not when you want them being answered correctly and exhaustively.

AMINATOR

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Re: OTC MDMA is now easy and cheap!!
« Reply #18 on: July 15, 2001, 02:04:00 AM »
O.k. I'm sorry, I guess maybe I'm a little over confident about my Ideas.All I have of chemistry knowledge, really is chemistry 20. I will be taking chem 30 next and eventually I will be enrolled in a chemical technology program. But I would surmise that its mostly because I love da Hive and beeing part of it. The Hive has sparked my interest in chemistry and thus it has been my decision to persue it as a proffesional career. Thanx everyone

PolytheneSam

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Re: OTC MDMA is now easy and cheap!!
« Reply #19 on: July 15, 2001, 02:49:00 AM »
Iodosafrole is supposed to be more reactive than the bromide according to some people.  I thought about this earlier, US patent 1380951 discloses a process for making HI from I2 using a terpene like pinene.  It sounds similar to the tetralin process.  Turpentine is mostly pinene.  Also, about the metallic sodium, I made some before using molten NaOH which is easily melted in an evaporating dish heated using a heating mantel or hot plate.  I used nails as electrodes and a 12V battery charger.  After a while little beads of sodium formed which I stored under mineral oil. 


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