Isosafrole to MDP2P Reagents: - 1050g 30% H2O2 - 4630g CH2O2 - 1000g isosafrole - 3700ml acetone - 1850ml MeOH - 11100ml

15% H2SO4 (905ml conc. H2SO4 in 10195ml H2O) - 6600ml Et2O

To a well stirred solution of 1050g of 30% hydrogen peroxide in 4630g 80% formic acid there was added, dropwise, a solution of 1000g isosafrole in 3700mL acetone at a rate that kept the reaction mixture from exceeding 40 C. This required a bit over 1 h, and external cooling was used as necessary. Stirring was continued for 16 h, and care was taken that the slow exothermic reaction did not cause excess heating. An external bath with running water worked well. During this time the solution progressed from an orange color to a deep red. All volatile components were removed under vacuum which yielded some 1850g of a very deep red residue. This was dissolved in 1850mL of MeOH, treated with 11100mL of 15% H2SO4, and heated for 3 h on the steam bath. After cooling, the reaction mixture was extracted with 3x 2200mL Et2O, the pooled extracts washed first with H2O and then with 5% NaOH, and the solvent removed under vacuum The residue was distilled (at 2.0 mm/ 108-112 C, or at about 160 C at the water pump) to provide 636.2g of 3,4methylenedioxyphenylacetone as a pale yellow oil.

MDP2P to MDMA using CTH with 10% Pt/C Reagents: - 2500ml MeOH containing 387.5g methylamine - 375g Glacial Acetic Acid - 1000g MDP2P - 62.5g 10% Pt/C - 3250ml Et2O - 250g anhydrous silica - Mol. Sieve 3A or MgSO4 - 25% NaOH Solution

The GAA/MeOH/MeAm were combined and the MDP2P was added dropwise with stirring. When addition was complete 250g of anhydrous silica gel was added and overhead stirring was commenced for 6 hours. The silica gel was ltered off and 62.5g of 10% Pt/C was added to the mix. This was then placed in a hydrogenator and shaken for 4 hours, at which point 105% of the theoretical H2 had been absorbed. The mix was ltered once with vacuum to recover the catalyst (which was rinsed with MeOH), and again through celite to remove the brackish color present due to remaining catalyst particles. 2500ml of the solution was placed in a 5L distillation apparatus and 1250ml of MeOH was removed at atmospheric pressure, after cooling, the remainder of the mix was added, and distilled until the temperature rose to 80C. After cooling, distillation was commenced again, collecting the acetic acid fraction. The residue was suspended in 3125ml water, basied with 25% aqueous NaOH, extracted with 3x 1000ml ether, the etheral solution dried and the ether distilled off under vacuum, and the residue was vacuum distilled, collecting 875ml of MDMA. The MDMA was taken up in 1250ml of ether and saturated with HCl gas until crystalization had ceased. The total quantity of hydrochloride salt recovered was 1096g. Recrystallization was done from MeOH, then after the fridge precitipation the MeOH was slowly evaporated to make big rocks. Theoretical yield from isosafrole: 69.7%