Does anyone here have a back up or possibly the site where a file was posted that was titled "OTC MDA Synthesis"

It was basically a reductive amination.

It went like:
Bubbling Chlorine gas through NaBr in a distilled water solution to get bromine.
Then adding bromine to Napthalene and letting the Hbr bubble through the safrole to yield bromosafrole.
And the the reductive amination. Methyamine (MDMA) (Or Ammonia for MDA) bubbled through ethanol and then the bromosafrole is added.


Any help to this file will be greatly appreciated. I have googled endlessly.

If you have a back up you can email it to me @ pyropeanut1776@gmail.com

After a grueling search effort. I have found it. If anyone would like me to send it to them I will.

After a grueling search effort. I have found it. If anyone would like me to send it to them I will.

Share the wealth man!

dreamalot11@hotmail.com

I'll post it to get some feedback from people. The part that is missing is just obtaining bromine. But I would use the method that I found easiest. Using sodium hypochlorite and HCl in a gas generator to bubble Chlorine gas through NaBr solution (aq) and then use a separatory funnel to remove the bromine.
OTC MDA/MDMA Synthesis.

I don't really love how this guy worded everything but it is really simple synth.

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

Pop the bromine/catalyst solution into the bottle.

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.

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.

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.


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

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.
Setup up the gas generator, 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:

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.

Why fuck around with chlorine when 2NaBr+H2SO4==>Na2SO4+2HBr?

EDIT: And what's this about a lewis acid? Your goal isn't to brominate the aromatic; it's to add HBr to the alkene! You'd be wasting your time attempting an aromatic halogenation to get HBr, besides, any FeBr3 left in the napthalene solution would likely add to your safrole giving you brominated shit. This write-up is poorly thought-out.

http://www.totse.com/community/showthread.php?t=2056615
http://designer-drugs.com/pte/12.162.180.114/dcd/chemistry/halosafrole.txt

But assuming you've got safrole, one would hope you'd put it to use in a way you'd receive decent yields. Whats so hard about an oxidation and amination?

-F☺rd

This doc seems more interesting simply regarding the production of HBr; rather then the actual promination they discuss here.

http://www.totse.com/community/showthread.php?t=2056615
http://designer-drugs.com/pte/12.162.180.114/dcd/chemistry/halosafrole.txt

But assuming you've got safrole, one would hope you'd put it to use in a way you'd receive decent yields. Whats so hard about an oxidation and amination?

-F☺rd


This one looks promising.

When he is talking about the two pathways for HBr to react, is he saying that it's better to not distill your oil?

This one looks promising.

When he is talking about the two pathways for HBr to react, is he saying that it's better to not distill your oil?

I've read that a few times, IIRC the suggestion that other compounds in the raw sassafras oil prevent free radical oxidation or somesuch 'bad things' which would otherwise dick with your yields, but it seems to be jsut a 'theory' thing, every time I've seen practical results its always yielded better with distilled and purified safrole.

I've read that a few times, IIRC the suggestion that other compounds in the raw sassafras oil prevent free radical oxidation or somesuch 'bad things' which would otherwise dick with your yields, but it seems to be jsut a 'theory' thing, every time I've seen practical results its always yielded better with distilled and purified safrole.

Yeah, I reread it he's trying to suggest that eugenol will prevent free radicals.

Wait a minute won't the H2SO4 oxidize the HBr to elemental Bromine?

2HBr + H2SO4 }}} Br2 + SO2 + 2H2O

Wait a minute won't the H2SO4 oxidize the HBr to elemental Bromine?

2HBr + H2SO4 }}} Br2 + SO2 + 2H2O

You have hit the nail on the head with that one - At least, I assume you're talking about NaBr/DMSO/H2SO4 method for brominating safrole - In which, yes, that's the case, and was why many bees and otherwise widely denounced that process after winding up with a whole pile of crap at the end of the rxn - The trick is to use a much lower concentration of H2SO4, about 65-70%; experiment to get the balance between speed of rxn and final yield.

You have hit the nail on the head with that one - At least, I assume you're talking about NaBr/DMSO/H2SO4 method for brominating safrole - In which, yes, that's the case, and was why many bees and otherwise widely denounced that process after winding up with a whole pile of crap at the end of the rxn - The trick is to use a much lower concentration of H2SO4, about 65-70%; experiment to get the balance between speed of rxn and final yield.

Thanks, My DMSO is gonna love you :p

You have hit the nail on the head with that one - At least, I assume you're talking about NaBr/DMSO/H2SO4 method for brominating safrole - In which, yes, that's the case, and was why many bees and otherwise widely denounced that process after winding up with a whole pile of crap at the end of the rxn - The trick is to use a much lower concentration of H2SO4, about 65-70%; experiment to get the balance between speed of rxn and final yield.


Man, I like this method but I don't want to hurt my precious root beer. I'm gonna be scared during this rxn.