The hypothetical synthesis shown below is what I have combined out of Bright Star's excellent piece of work and Dr. Gonzo's awesome nitromethane route to the finished product.
Distillation of Sassafras oil to yield pure Safrole
Under vacuum, slowly raise heat until Safrole starts coming over; record temperature
Switch flasks and then heat to ~10° under where the Safrole came over
RXN: Wacker Oxidation of Safrole -> MDP-2-P
In a 500mL RBF, put 300mL DMF, 50mL H2O, 120g p-Benzoquinone, and 2g PdCl2
Start magnetic stirrer on slow
Mix 160g Safrole and 50mL DMF and drip into the flask over 30 minutes
Solution should turn a very dark red-orange
Continue stirring for 7 hours
Flood rxn mix with slightly acidic water and mix contents thoroughly
Decant organic layer and save
Wash aqueous layer with 2x100mL DCM and save
Combine organic layer and DCM washes and wash with 2x150mL 10% NaOH
Decant organic layers and save
Distillation of rxn contents to yield pure MDP-2-P
In a 500mL RBF goes the impure MDP-2-P and boiling stones
Weigh receiving flask and set up to vacuum distill
Turn up the heat to where the Safrole came over under vacuum
Release vacuum and replace receiving flask; start vacuum slowly
Maximum theoretical yield ~120g pure MDP-2-P (?)
RXN: Al/Hg/Nitromethane Amalgam of MDP-2-P -> MDMA
On a 2L 3-necked RBF, plug one neck and place a condenser in the center neck
Prepare 27.5g Al foil and add to flask
Dissolve 400mg HgCl2 in 750mL MeOH
Mix 25g MDP-2-P, 20g Nitromethane, and 25mL MeOH in addition funnel
Pour the MeOH solution into the flask and turn on the condenser
Open valve on addition funnel to about 1 drop a second
Stir briefly every minute
After the flask starts heating up, leave the stirrer on continuously
Adjust the flow rate of the funnel accordingly
When the rxn starts to slow down, add another 75mL of MeOH and let sit for about an hour
Mix 700mL H2O and 262g NaOH in a beaker
Dump the rxn contents into a 4L beaker (add MeOH to loosen sludge)
Add the NaOH solution to the beaker
Stir the mixture for about an hour
Add 500mL toluene and stir for a few minutes, then layer
Wash the sludge with 2x250mL toluene and save
Combine toluene layers
Wash 2x with saturated Sodium Bicarbonate, once with saturated NaCl, and once with H2O
Drain into an extremely clean beaker with 35g anhydrous MgSO4, stir, and let sit for 30 minutes
Filter into a very clean beaker and wash the MgSO4 with a little more toluene
Gas with anhydrous HCl until MDMA precipitates out of solution
When solution becomes cloudy, cover the beaker and place in the freezer for half an hour
Vacuum filter
Continue to gas the toluene until no there is no more MDMA precipitate
Chill, filter, and dry
Maximum theoretical yield ~90g pure MDMA (?)
I have a few unanswered questions, though.
Can I use Xylene instead of toluene? Are there any other chems that I could substitute with more OTC products? Any advice on the best way to get ice-cold water running through your condenser, instead of just cold tap-water? I'm trying to eliminate variables so I can come up with a good 'hypothetical' yield the first time, so any corrections/additions/etc. would be helpful.
Any comments on this would be greatly appreciated.