MDMA synthesis from piperonylmethylketone (PMK/MDP2P) with formic acid

[IM BATMAN]

found this awesome BIG scale MDMA via leuckart, it explain some more steps, but there are things i dont understand yet.... in the step 1 iT saYS: " Add the 20 L extra oil to the 160 L = 180 L." i dont understand that number, since they start from 150L ...I SUPPOSE its the mixing result that this Friend names just OIL



This method is used in the past in Europe on huge scale to make MDMA:

[1] 150 L MDP2P + 400 L NMF + 75 L Formic acid :

heat to 190°C (at 140°C H2O + Formic acid comes over) for about 6 Hrs. until
smell of Ammonia-gas is present at the collecting flask. No vacuum! Let cool and
wash with 350 L water to get rid of excess NMF. Tap off 160 L oil and extract
the remaining water with 2 x 30 L DCM. Cook off that DCM at 60°C and 200 mm Hg.
Add the 20 L extra oil to the 160 L = 180 L.

[2] Cook with HCl : Hydrolysis.

180 L oil + 100 L methanol + (250 L HCl 36% + 550 L H2O): Mix and cook. At 60-65°C
MeOH distills over, after that go to 95 C and stay there for 3 Hrs. You make now
the chloride salt, which dissolves in the water part. Let cool off to 40°C and
extract with 40 L DCM. THROW AWAY THE DCM extract, this is full of impurities.
KEEP the water-part!

[3] Making Basic.

100 Kg NaOH dilute in 100 L water (90 L 100% HCl needs +/- 70 L NaOH). Use this
NaOH solution to basify the remaining water portion. DO NOT exceed 40C! Bring to
pH 10.3 and then +/- 100 L MDMA base oil will come. Extract with 2x30 L DCM and
distill off the DCM to get raw base.

[4] Distillate.

At 4 mm Hg (or any other good vacuum) and 145°C you distillate the raw base to
get the clean base. (first remove DCM and water).

[5] Crystalls.
If you know my name now, search my posts how to make them.... Use Acetone cold
and HCl gas...

 

[IM BATMAN]

at the end, in the Crystallization step, he say " use acetone cold and HCL gas.... if i understood, it means treat the crude base MDMA dissolved in Cold acetone then GAS? i know the hcl salt does not dissolve in Acetone but maybe the base does... or he means treat the base goo dissolved in methanol, gased and then crystallized in cold acetone? it sounds more logic to me

 

[Mclssmxxl]

I think you are correct.Distill crude product -> Get pure product -> Dillute with cold aceton -> Gas the aceton solution.
I don’t have first hand experience working up md but this is the way it makes sense the most.

 

[IM BATMAN]

Tnx friend , i'll try for sure!

 

[G.Patton]

Hello, no. You won't get MDMA. You'll get MDA probably but I'm not sure.

 

[RA!NER]

How many diethylether how many methanol how many aceton?

 

[G.Patton]

2 x50 mL
as small as possible to dissolve it
approximately 1.5 volume of methanol

 

[RA!NER]

Thank you

 

[ossi]

please please video

 

[RA!NER]

Guys I need some expert advice from you. I have taken up my very first work with no prior experience. I was able to successfully make PMK oil and started the actual synthesis as described above only multiplied the amount by 10. Refluxed with formic acid and N-MF and PMK for seven hours. After that it cooled down a bit so that it did not bubble anymore (but not room temperature) and I added the hydrochloric acid. Refluxed for another three hours. Then I added enough NAOH to get a PH value of 12. So far so good. I added diethyl ether and separated the reaction mass so that the ether was also separated. Then I got into trouble because I did not write down that the ether should remain with the freebase. The second problem was how much magnesium sulfate to use. I crushed dried sulfate and added too much to the freebase. The next day I saw a large white amount and some brown liquid floating on top, I didn't know there anymore what my target substance was respectively I didn't know what I had to process further. First I made a warm water bath and put the vessel in it to evaporate the sulfate. I thought that what would be left would be my freebase. But that didn't happen. So I heated the amount to 100 degrees hoping to evaporate sulfate. Nothing happened except steam that smelled heavily of anise, almost like marzipan but no sulfate. There remained a white mass that also smelled of anise. Then I put hydrochloric acid in a new container, dripped sulfuric acid in to produce the reaction to HCL gas. This didn't happen either so I heated the acids and directed the vapor into the white mass. Bubbles everywhere but the color did not change to brown. It remained white. I filtered it with with the Buchner vacuum filter and smeared the amount into a bowl. I followed the recipe and heated methanol to 50 degrees. Then I put the methanol on the slime and stirred it to dissolve it. I let it cool to 25 degrees and put cold acetone from the refrigerator on top. Condition: White paste below liquids above. I dumped the liquids after a while and put the bowl in the container to vacuum. Slowly, after bubbling, not much was happening. So I wanted to re-crystallize the amount. Poured it into a beaker and heated it to 150 degrees. Nothing more happened. I let it cool and put it aside airtight.

 

[Curiousonion]

"Then I got into trouble because I did not write down that the ether should remain with the freebase."

What do you mean by that, what did you to after you collected the ether with the freebase? Did you add the magnesium to the ether?

 

[RA!NER]

i seperated the ether from the freebase and after that I dried the freebase with the magnesium

 

[Curiousonion]

Well that's the problem. You supposed to dry the solvent containing the freebase.
So either dry the ether with the freebase or the acetone in which you are going to mix the freebase in before gassing.

 

[RA!NER]

So what can I do now any steps to safe some mass ?

 

[Curiousonion]

Well I don't know how badly you messed around with the freebase but if it only has dry magnesium in it I would mix it into anhydrous acetone then gas it.

 

[RA!NER]

Well thanks I will try

 

[RA!NER]

You me
an heating or distill or hcl Gas?

 

[Curiousonion]

Not sure i understand your question.
But technically you should have a gummy mass of freebase mixed with magnesium salts.
Take that and mix it with anhydrous acetone.
Then Remove the magnesium which will separate and fall to the bottom.


then use a gas bubbler on it.

 

[G.Patton]

Agree. I don't understand why @RA!NER decided to heat this mixture. There is no solvent. MgSO4 will not melt. You just need to add same amount of ether as for extraction and remove MgSO4 via filter. Than, wash MgSO4 by solvent couple times to collect all free base.

Probably, you will lost part of reaction yield.

 

[RA!NER]

Alright I will do this - any other opportunity to extract cause im out of diethylether ?