MDMA by Catalytic Hydrogenation of MDP2P and Methylamine
Using Platinum on Carbon (10%) Catalyst – by KrZ
Reactants
- 4L MeOH containing 620g (20 mol) Methylamine
- 600g (10 mol) Glacial Acetic Acid
- 1600g MDP2P
- 100g 10% Pt/C
The GAA/MeOH/MeAm were combined and the MDP2P was added dropwise with stirring. When addition was complete 400g of anhydrous silica gel was added and overhead stirring was commenced for 6 hours. The silica gel was filtered off and 100g 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 filtered 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. 4L of the solution was placed in a 5L distillation apparatus and 2L of MeOH was removed at atmospheric pressure, after cooling, the remainder of the mix was added, and distilled until the temperature rose to 80°C. After cooling, distillation was commenced again, collecting the acetic acid fraction. The residue was suspended in 5L water, basified with 25% aqueous NaOH, extracted with ether, the etheral solution dried over MgSO4, the ether distilled off under vacuum, and the residue was vacuum distilled, collecting 1400ml of MDMA. The MDMA was taken up in 2L of ether and saturated with HCl gas until crystalization had ceased. The total quantity of hydrochloride salt recovered was 1755g.
Using Platinum(IV)oxide Catalyst – by LaBTop
Reactants
- 1800 ml MDP2P
- 1200 ml Methanol
- 1200 ml (1080g) anhydrous liquid MeNH2 (bp -6°C!)
- 24 g Platinum(IV)oxide (Adam’s Catalyst)
Switch your vacuumpump on, connected by valve to the system. First you mix the PtO2 with the MDP2P, because this can not catch fire! Then you fill this mix in your clean and evacuated hydrogenator, with the help of a deep stainless steel funnel with a valve under it, welded on top of your hydrogenator. Fill the funnel and let the mixture be sucked in, but not completely, close valve and fill funnel again, etc. Let no air come in. Then you fill the cold liquid methylamine through your stainless steel flexible hose, preferable also with a valve inbetween (Valves are a necessary safety precaution for pressure bombs, they tend to become BOMBs when oxygen comes into the reaction). Do not forget to vacuum the stainless steel hose up till the gas-cylinder too, before you let the MeNH2 in. As the last you fill the Methanol through your stainless steel funnel. You close all valves, except the valve to the H2 cylinder (evacuate the stainless steel pipe to the hydrogen cylinder too). Stop your vacuum pump (after closing its valve!). Now you warm up the hydrogenator to 50-55°C and keep it there. Open the H2 gas valve and bring the whole thing to 3.5 atm, not higher or lower! Keep it there! Now you start the mixer (Not earlier, or poisonous byproducts will be formed and influence the reaction badly). Let react for 30 minutes. During this time the temp. will rise 5-9°C. As soon as the temp. drops 3-5°C the reaction has ended (about 30 min). Let off the pressure and evacuate the last amount of hydrogen using your vacuum pump, and then you let clean air into the system. Now you tap off your raw MDMA freebase in a metal bucket (it’s hot you know), filter and vacuum distill it, then make crystals using HCl. Re-use your PtOIV! Yes, 1:1,1.
A good extra read is «Home Hydrogenation» by Popeye. He gives a lot of small details which you surely should read.
Using Platinum(IV)oxide Catalyst – by Simulator
If the clandestine chemist would make MDMA, he would use a low-pressure stainless steel autoclave with 1/4 space for the Hydrogen gas, a mixer motor on top and the shaft made leakproof by a mechanical seal to stand 5.0 bar pressure and about 0.5 bar vacuum. In a large freezer he should cool the big steel cylinder of methylamine gas to it condenses to a liquid (bp -6°C), and he should lift the cylinder with a (takel zoals gebruikt in garages) in a near horizontal position just till above the fridge. With a flexible stainless steel hose is the cylinder conected to the autoclave, between the sealing and the lift he would make a scale to be able to weigh te amount of gas he should use.
Reactants
- 1500 ml MDP2P
- 1000 ml Methanol
- 1100 ml (990g) anhydrous liquid MeNH2 (bp -6°C!)
- 10 g Platinum(IV)oxide (Adam’s Catalyst)
When those chemicals are in the autoclave he will evacuate the autoclave to a vacuum of approx. 0.5 bar to get rid of the oxygen. Then he should open the hydrogen bottle for a short moment till approx. 1.0 bar,and then evacuate a second time to be absolute sure all the oxygen is out.
He should then start the mixer motor (brush-less type in case of a hydrogen leak) and then he should pressurize with hydrogen to approx. 3.5 bar. By adjusting the pressure between 2.5-4.0 bar he could keep the temp. around 50°C and never higher than 60°C. After ca 2 hours the temp will possibly go down, to control the uptake of the hydrogen gas he should close the bottle and watch for a period of 10 minutes if the pressure in the autoclave gets lower. In that case open up the hydrogen bottle for a few minutes more and otherwise the reaction is stopped, and he could after a couple of hours drain the autoclave. He should use a Buchner filter on a vacuum bottle with Whatman no 401 filtering paper, he expect that other type of filters makes this filtering of the Platinum powder a endless job. He would then distill off the MeOH, the MeNH2 and the water at atmospherical pressure. He then changes the recieving flask and at about 150-160°C at 20 mmHg vacuum the MDMA freebase oil will come over in approximately 90% yield (depends on the purity of the MDP2P). For making the MDMA hydrochloride crystals he bubbles dry HCl gas through a solution of 1000ml freebase in 7-8 L chilled (4°C) diethyl ether, and filters off the precipitated crystals to get 1100g MDMA hydrochloride after drying.
Note that this reaction is not possible to perform with 40% aqueous methylamine.
