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.
blah blah blah something clever blah blah blah