Синтез МДМА из сафрола
через бромопроизводное.
1. Бромирование.
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 (см также альтернативные методы получения
бромоводорода)
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:
3. Экстракция.
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.