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



## William Dampier

*Reaction scheme:*


​*Equipment and* *glassware**:*

100 ml round bottom flask;​
Retort stand and clamp for securing apparatus (optional);​
Reflux condenser;​
Heating plate;​
Funnel;​
Syringe or Pasteur pipette;​
pH indicator papers;​
Beakers (250 mL x2, 100 mL x4);​
Vacuum source;​
Laboratory scale (0.01-100 g is suitable);​
Measuring cylinders 10 mL and 100 mL;​
Water bath;​
Glass rod and spatula;​
Separatory funnel 0.5 L;​
Laboratory grade thermometer (up to 200-250 °C); ​
Buchner flask and funnel; ​
Filter paper;​

*Reagents:*

Formic acid 10.98 g;​
n-Methylformamide (NMF; cas 123-39-7) 7.6 g;​
MDP2P (PMK; cas 4676-39-5) 9.0 g;​
Concentrated hydrochloric acid (HCl 36%) 30 ml;​
Sodium hydroxide solution (NaOH 35%) ~10 ml;​
Diethyl ether (or petroleum ether) ~150 ml;​
Magnesium sulphate (MgSO4) ~15 g;​
Methanol (MeOH) ~50 ml;​
Acetone ~50 ml;​

*Synthesis:*
*1.* Formic acid 3.66 g, n-methylformamide (NMF) 7.6 g and MDP2P (PMK) 9.0 g are placed into a 100 ml round bottom flask. Reflux condenser and thermometer are installed.
*2.* The mixture is refluxed at 150-170 °C for 7 h with periodic formic acid 7.32 g additions.
*3.* After that, the reaction mixture is cooled down to room temperature, a clear yellow solution of N-formyl-3,4-methylenedioxymethylamphetamine (N-formyl-MDMA) is obtained. N-formyl-MDMA solution have to be washed with distilled water twice and dried over MgSO4. Dry solution is filtered from solids.
*4.* Concentrated hydrochloric acid (HCl 36% 30 ml) is added to this solution. Than, reaction mixture is heated at 80 °C for additional 3 h.
*5.* The reaction mixture is alkalized with several portions of sodium hydroxide solution (NaOH 35%) to 12 pH. Do not overheat reaction mixture.
*6.* Crude MDMA free base is extracted from the alkaline solution with diethyl ether (or petroleum ether) 2 x 50 mL. Ether extract with MDMA free base is dried over MgSO4. 
*7.* After that, organic solvent is evaporated with a slight heating of warm water bath or with help of rotary evaporator with vacuum. MDMA free base oil is treated with hydrogen chloride gas and gelatinous brown precipitate of impure MDMA hydrochloride is obtained.
*8. *The crude MDMA hydrochloride salt is dissolved in minimum volume of boiling methanol (MeOH), which is necessary to dissolve MDMA crude salt. Hot solution is poured into a beaker with chilled acetone, crystals are formed. This mixture is cooled down to a room temperature and vacuum filtered, crystals are washed with small amount of cold dry acetone and air dried (or dried in a vacuum chamber). Crystalline MDMA hydrochloride is obtained as the product.
*9. *MDMA hydrochloride can be recrystallized one more time to yield fawn crystals with melting point 147 - 148 °C.​


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## Honolulu98

William Dampier said:


> *Reaction scheme:*
> View attachment 1473
> 
> *Synthesis:*
> 1. Formic acid (3,66 g), NMF (7,6 g) and PMK (9.0 g) were refluxed at 150-170 *C for 7 h with additional formic acid (7,32 g) added periodically.
> 2. On cooling, a clear yellow solution of N-formyl-3,4-methylenedioxymethylamphetamine (N-formylMDMA) was obtained.
> 3. Concentrated hydrochloric acid (30 ml) was added to this solution, which was refluxed for a further 3 h.
> 4. The reaction mixture was made basic with sodium hydroxide, and the crude MDMA extracted into diethyl ether.
> 5. After the volume of the organic solvent was decreased, the remaining residue was treated with hydrogen chloride gas to yield a gelatinous brown precipitate of impure MDMA hydrochloride.
> 6. The crude salt, dissolved in boiling methanol, was added to chill acetone to form a crystalline product.
> 7. This was recrystallized to yield fawn crystals with a melting point of 147 - 148 *C.



William Dampierif possible use DMF or is better NMF?


Any difference?


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## William Dampier

No, DMF is impossible for this reaction


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## rickyrick

What in your opinion is the best way to get or synthesise PMK at this day and age?PMK methyl glycidate maybe?


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## William Dampier

Definitely PMK-gly is the best source (after sassafras oil, if you can buy it)


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## Gale

This method seems really nice, but how are the yeilds?


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## blackchip

what does it mean to treat with hydrogen chloride gas?


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## William Dampier

blackchip said:


> what does it mean to treat with hydrogen chloride gas?



blackchipWith a gas generator. But you can use aqueous hydrochloric acid and dry acetone.


Gale said:


> This method seems really nice, but how are the yeilds?


At best, the same amount as PMK-oil, in the form of hydrochloride, but rather less.


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## Followme38

Can you use standard formamide instead of nmf ?


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## blackchip

William Dampier said:


> With a gas generator. But you can use aqueous hydrochloric acid and dry acetone.



William Dampier
I am sorry for asking this question again but I read the literature on the hcl gas generator but it doesn't answer my question. If I make the gas with the generator, does 'treating' mean passing the gas through a flask with the crude MDMA?


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## Followme38

blackchip said:


> I am sorry for asking this question again but I read the literature on the hcl gas generator but it doesn't answer my question. If I make the gas with the generator, does 'treating' mean passing the gas through a flask with the crude MDMA?



blackchipJust use anhydrous acetone and 37% hcl working with hcl gas is dangerous as hell  and there is not advantage if you crystal in fridge


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## Gale

Followme38 said:


> Just use anhydrous acetone and 37% hcl working with hcl gas is dangerous as hell  and there is not advantage if you crystal in fridge



Followme38You mean to add 37% hcl dropwise to anhydrous acetone till acidic then freeze? Gassing isn't that dangerous if done properly, its really chill. Just not the most comfortable, I would rather have a dry acidic solution I could add to the NP, such as sulfuric acid. Would be smoother. Will it be ok to go the sulphate route? I have a feeling it will make some pretty crystals


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## Followme38

Gale said:


> You mean to add 37% hcl dropwise to anhydrous acetone till acidic then freeze? Gassing isn't that dangerous tbh and with proper exhaust you can even take your mask off.
> 
> Gassing seems to be the best option and will cut down on time and solvents.



GaleYou are right at this point only its hard to get your hands on gas most of the time


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## Gale

Followme38 said:


> You are right at this point only its hard to get your hands on gas most of the time



Followme38Unless you live in most places where its the easiest reagent to access. HCL aq poured on calc chloride = gasolina


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## Montecristo

hey, What is the formic acid concentration?
So instead of gassing i would wash the residue with hcl and acetone?
Is there alternative to diethyl ether? can i use DCM? or Naptha?
And do i have to convert the new [Ethyl Gylc] PMK into PMK oil?
Thanks!



William Dampier said:


> *Reaction scheme:*
> View attachment 1473
> 
> *Synthesis:*
> 1. Formic acid (3,66 g), NMF (7,6 g) and PMK (9.0 g) were refluxed at 150-170 *C for 7 h with additional formic acid (7,32 g) added periodically.
> 2. On cooling, a clear yellow solution of N-formyl-3,4-methylenedioxymethylamphetamine (N-formylMDMA) was obtained.
> 3. Concentrated hydrochloric acid (30 ml) was added to this solution, which was refluxed for a further 3 h.
> 4. The reaction mixture was made basic with sodium hydroxide, and the crude MDMA extracted into diethyl ether.
> 5. After the volume of the organic solvent was decreased, the remaining residue was treated with hydrogen chloride gas to yield a gelatinous brown precipitate of impure MDMA hydrochloride.
> 6. The crude salt, dissolved in boiling methanol, was added to chill acetone to form a crystalline product.
> 7. This was recrystallized to yield fawn crystals with a melting point of 147 - 148 *C.



William Dampier



William Dampier said:


> *Reaction scheme:*
> View attachment 1473
> 
> *Synthesis:*
> 1. Formic acid (3,66 g), NMF (7,6 g) and PMK (9.0 g) were refluxed at 150-170 *C for 7 h with additional formic acid (7,32 g) added periodically.
> 2. On cooling, a clear yellow solution of N-formyl-3,4-methylenedioxymethylamphetamine (N-formylMDMA) was obtained.
> 3. Concentrated hydrochloric acid (30 ml) was added to this solution, which was refluxed for a further 3 h.
> 4. The reaction mixture was made basic with sodium hydroxide, and the crude MDMA extracted into diethyl ether.
> 5. After the volume of the organic solvent was decreased, the remaining residue was treated with hydrogen chloride gas to yield a gelatinous brown precipitate of impure MDMA hydrochloride.
> 6. The crude salt, dissolved in boiling methanol, was added to chill acetone to form a crystalline product.
> 7. This was recrystallized to yield fawn crystals with a melting point of 147 - 148 *C.


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## Montecristo

How much hcl and dry acetone should be used?
what is yeild compared to bubbling hcl?


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## Gale

thatfella said:


> How much hcl and dry acetone should be used?
> what is yeild compared to bubbling hcl?



thatfellaYeild should be the same and IMO gassing is the best method whether you perform this step directly or after collecting and drying out base, then dissolve in IPA and maybe add a few mls hcl aq and freeze..which should give you some crystals..but id reccomend to gas a bunch of IPA and save it. Then you have dry IPA/HCL. Whenever you need it, its ready and all you have to do is add HCl/IPA to dry NP to pH 5?

The gassing stage is really the most relaxing step. It seems intimidating but with good exhaust airflow you don't even need to wear a mask IME, I take mine off sometimes and I dont smell a thing...might be smart to wear protective face sheild for w.e reason the tube gets clogged and pressure builds up and escapes in random direction.


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## Gale

thatfella said:


> How much hcl and dry acetone should be used?
> what is yeild compared to bubbling hcl?



thatfellaYeild should be the same and IMO gassing is the best method whether you perform this step directly or after collecting and drying out base, then dissolve in IPA and maybe add a few mls hcl aq and freeze..which should give you some crystals..but id reccomend to gas a bunch of IPA and save it. Then you have dry IPA/HCL.. IMO it feels more organised to me when using dry IPA/hcl..no need for setting up for gassing or waiting for the right time to gas etc.

The gassing stage is really the most relaxing step. It seems intimidating but with good exhaust airflow you don't even need to wear a mask IME, I take mine off sometimes and I dont smell a thing...might be smart to wear protective face sheild for w.e reason the tube gets clogged and pressure builds up and escapes in random direction, which could blind u or give u a nice burn... With that in mind, gassing is still a relaxing and easy process.


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## Montecristo

Yeah sweet, i am aware of how to gas HCL to get a higher concentration acid using Azeotrope distillation, is this the same method with the gas line going into solution?


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## Montecristo

do you just gas until all the product has crystalized?


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## Montecristo

how do you use gassed IPA in this situation? How do you know when the ipa has been gassed enough?


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## Gale

thatfella said:


> do you just gas until all the product has crystalized?



thatfellaI gas until I feel its ready, still dialing that. You should bring PH to 5 I believe and then freeze for a few hours.

IPA/HCL will give u same results as gassing at the end if the day, should wash with acetone afterwards anyway.


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## Gale

thatfella said:


> how do you use gassed IPA in this situation? How do you know when the ipa has been gassed enough?



thatfellaYou can weigh the IPA that is a great way to know the concentration. Weigh before and after gassing until lots of gas is escaping and not absorbing into solution.


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## Montecristo

so in all the above methods, HCL source should be added till pH 5?


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## Montecristo

Gale said:


> You can weigh the IPA that is a great way to know the concentration. Weigh before and after gassing until lots of gas is escaping the solution and not absorbing.



GaleOkay thank you. what would be a good concentration?


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## Gale

thatfella said:


> Okay thank you. what would be a good concentration?



thatfellaI can't recall the exact amount but might as well gas as much as you can or until lots of gas is eacaping and no longer absorbing into IPA. I think you want to aim for 20-30% by weight in HCl.


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## Montecristo

okay sweet, sounds the same as concentrating HCL acid. 
Thanks for the help.


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## Montecristo

If both methods work the same , wouldnt it save a fair a bit of time just using concentrated hcl and IPA?


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## blackchip

William Dampier said:


> *Reaction scheme:*
> View attachment 1473
> 
> The reaction mixture was made basic with sodium hydroxide, and the crude MDMA extracted into diethyl ether. After the volume of the organic solvent was decreased, the remaining residue was treated with hydrogen chloride gas to yield a gelatinous brown precipitate of impure MDMA hydrochloride.



William Dampier
After the crude mdma is extracted into the diethyl ether, do you vacuum distill off the ether?


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## William Dampier

blackchip said:


> After the crude mdma is extracted into the diethyl ether, do you vacuum distill off the ether?



blackchipThe product can crystallize in chilled ether


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## Montecristo

Any safety concerns on the use of this method?


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## William Dampier

thatfella said:


> Any safety concerns on the use of this method?



thatfellaCaution with hot liquids and pairs of formamide and hydrochloric acid. In general, there is no problem, classic Leuckart reaction.


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## PepitoPistol

William Dampier said:


> The product can crystallize in chilled ether



William DampierCan any other solvent be used for the extraction?
What's the expected yield of the method?
Dissolving in boiling methanol and quenching in cold acetone doesnt seem very practical from my perspective, because acetone is strictly regulated here. Could it be dissolved in IPA/HCl and cristallized in the freezer? Does it affect yields much?
Thanks!


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## Gus_Fring

I know this Method but..is not very good to be true? i mean... whats the trick? low yields maybe? i will try FOR SURE anyway


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## Montecristo

Would this method scale up safely? eg 10x or 20x?


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## RustyShackleford

William Dampier said:


> No, DMF is impossible for this reaction



William Dampier
Is that because the solvent will take place in the reaction and using DMF would produce MD-dimethyl-A? Both DMF and NMF are difficult to obtain directly for me, and from a quick glance at the preperation of formamide, it looks like I would need methylamine (or dimethylamine) to make them, at which point I feel like it's more practical to just create the imine and gas it with H2, so if I were to do this, I would want to choose an easier to obtain solvent.


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## Montecristo

What concentration of formic acid is used? anhydrous? or is 80-85% okay?


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## Bimbone

I really hope that this technique will make it possible to make worthy crystals, or at least similar


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## Fring

thatfellon said:


> What concentration of formic acid is used? anhydrous? or is 80-85% okay?



thatfellonthats a good question... hope the publisher help us.


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## William Dampier

Bimbone said:


> I really hope that this technique will make it possible to make worthy crystals, or at least similar



BimboneThis is one of the classic routes, everything works


thatfellon said:


> What concentration of formic acid is used? anhydrous? or is 80-85% okay?


Anhydrous formic acid u are unlikely to find. The reaction can be carried out without it, only with N-MethylFormamide


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## Saymynamehsb

Made a thread on how to press pills if someone succeeds in this syntheses
Cheapest way of Making Ecstasy pills from MDMA without a pill press


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## Montecristo

William Dampier said:


> This is one of the classic routes, everything works
> 
> Anhydrous formic acid u are unlikely to find. The reaction can be carried out without it, only with N-MethylFormamide



William Dampierawesome thank you!
Would this method scale up safely? eg 10x or 20x?


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## Montecristo

William Dampier said:


> This is one of the classic routes, everything works
> 
> Anhydrous formic acid u are unlikely to find. The reaction can be carried out without it, only with N-MethylFormamide



William Dampierhow much ether would be required ?


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## William Dampier

thatfellon said:


> awesome thank you!
> Would this method scale up safely? eg 10x or 20x?



thatfellonEven more. But I'd rather edit the proportions depending on how much PMK you do. For a large and small scale, the proportions may differ, in addition, there are a couple more features, such as the water content of solvents. If you have all the reagents, I am ready to help in PM, you can publish the results here, if you want


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## William Dampier

u can also try to find a methylammonium formate (dry), but not sure if it's available now.


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## btcboss2022

How much is the yield of that synth finally?
Thanks.


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## Fring

William Dampier said:


> This is one of the classic routes, everything works
> 
> Anhydrous formic acid u are unlikely to find. The reaction can be carried out without it, only with N-MethylFormamide



William Dampierbut a non anhydrous formic acid would work?


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## Montecristo

awesome thank you. I would want to do 90-100g pmk. I do not have the reagents yet , i am waiting on other ones for amphetamine sulfate then i will get onto the reagents needed for this. I will let you know, and i will document both synths and post here for everyone.



William Dampier said:


> Even more. But I'd rather edit the proportions depending on how much PMK you do. For a large and small scale, the proportions may differ, in addition, there are a couple more features, such as the water content of solvents. If you have all the reagents, I am ready to help in PM, you can publish the results here, if you want



William Dampier


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## Montecristo

first time i will do the synth size as above to get a better understanding/experience , but then i would want to do 10x .


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## William Dampier

btcboss2022 said:


> How much is the yield of that synth finally?



btcboss2022If we get a yield of salt 1g per 1g oil, this is a good result, but rather less.


Fring said:


> but a non anhydrous formic acid would work?


Yes, it catalyzes the process.


thatfellon said:


> first time i will do the synth size as above to get a better understanding/experience , but then i would want to do 10x .


Write me in PM when you are ready


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## daqwen

William Dampier said:


> *Reaction scheme:*
> View attachment 1473
> 
> *Synthesis:*
> 1. Formic acid (3,66 g), NMF (7,6 g) and PMK (9.0 g) were refluxed at 150-170 *C for 7 h with additional formic acid (7,32 g) added periodically.
> 2. On cooling, a clear yellow solution of N-formyl-3,4-methylenedioxymethylamphetamine (N-formylMDMA) was obtained.
> 3. Concentrated hydrochloric acid (30 ml) was added to this solution, which was refluxed for a further 3 h.
> 4. The reaction mixture was made basic with sodium hydroxide, and the crude MDMA extracted into diethyl ether.
> 5. After the volume of the organic solvent was decreased, the remaining residue was treated with hydrogen chloride gas to yield a gelatinous brown precipitate of impure MDMA hydrochloride.
> 6. The crude salt, dissolved in boiling methanol, was added to chill acetone to form a crystalline product.
> 7. This was recrystallized to yield fawn crystals with a melting point of 147 - 148 *C.



William DampierWhat are the volume measurements of each one?


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## Fring

thatfellon said:


> awesome thank you. I would want to do 90-100g pmk. I do not have the reagents yet , i am waiting on other ones for amphetamine sulfate then i will get onto the reagents needed for this. I will let you know, and i will document both synths and post here for everyone.



thatfellonplease bro.. kindly post here the results and the proccedure... i want to try this method as well, but since there are not much clear info would be freat if you can help us.


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## ADATA

Can 28281-49-4 be used as PMK?


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## daqwen

*Reaction scheme:*



William Dampier said:


> View attachment 1473
> 
> *Synthesis:*
> 1. Formic acid (3,66 g), NMF (7,6 g) and PMK (9.0 g) were refluxed at 150-170 *C for 7 h with additional formic acid (7,32 g) added periodically.
> 2. On cooling, a clear yellow solution of N-formyl-3,4-methylenedioxymethylamphetamine (N-formylMDMA) was obtained.
> 3. Concentrated hydrochloric acid (30 ml) was added to this solution, which was refluxed for a further 3 h.
> 4. The reaction mixture was made basic with sodium hydroxide, and the crude MDMA extracted into diethyl ether.
> 5. After the volume of the organic solvent was decreased, the remaining residue was treated with hydrogen chloride gas to yield a gelatinous brown precipitate of impure MDMA hydrochloride.
> 6. The crude salt, dissolved in boiling methanol, was added to chill acetone to form a crystalline product.
> 7. This was recrystallized to yield fawn crystals with a melting point of 147 - 148 *C.



William DampierWhat NMF means?


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## callmecharlie

daqwen said:


> *Reaction scheme:*
> 
> What NMF means?



daqwen
N-Methylformamide
CAS: 123-39-7


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## PepitoPistol

thatfellon said:


> first time i will do the synth size as above to get a better understanding/experience , but then i would want to do 10x .



thatfellonDid you try this?
Can you share some results? I’m deciding which way to go, but there’s too little info…
Thanks!


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## daqwen

Can someone explain me the instrucion 5 and 6? Can Somenone explain with more details?


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## MadHatter

daqwen said:


> Can someone explain me the instrucion 5 and 6? Can Somenone explain with more details?



daqwen*5. After the volume of the organic solvent was decreased, the remaining residue was treated with hydrogen chloride gas to yield a gelatinous brown precipitate of impure MDMA hydrochloride.*

Organic solvents can mostly be evaporated by low heating. It means you reduce the volume of the remaining solution by gentle heating. When you're left with something like half the original volume, you set up a HCl gas generator. This is done by dripping concentrated sulphuric acid onto table salt and passing the fumes that are produced (dry HCl gas) via a tube into the solution to bubble. You can find a detailed description of how to construct a HCl gas generator under "laboratory techniques" on this forum. 
Once the HCl gas bubbles into the solution, a brown gel is formed: this is the product. Once no more goo is being formed when you bubble gas into the solution, the reaction is finished and you can filter out the brown goo.

*6. The crude salt, dissolved in boiling methanol, was added to chill acetone to form a crystalline product.*

The "crude salt" is the brown goo. Pour it into some boiling methanol under stirring. When all is dissolved, let chill down for a bit and then pour the mix into ice cold acetone. NOW you'll get the nice MDMA crystals.


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## MadHatter

Also, before you pour everything into ice cold acetone, make sure it's well below 50 degrees C. Acetone boils at 56 degrees, and if you dump a boiling hot solution into it ...


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## IM BATMAN

DocX said:


> *5. After the volume of the organic solvent was decreased, the remaining residue was treated with hydrogen chloride gas to yield a gelatinous brown precipitate of impure MDMA hydrochloride.*
> 
> Organic solvents can mostly be evaporated by low heating. It means you reduce the volume of the remaining solution by gentle heating. When you're left with something like half the original volume, you set up a HCl gas generator. This is done by dripping concentrated sulphuric acid onto table salt and passing the fumes that are produced (dry HCl gas) via a tube into the solution to bubble. You can find a detailed description of how to construct a HCl gas generator under "laboratory techniques" on this forum.
> Once the HCl gas bubbles into the solution, a brown gel is formed: this is the product. Once no more goo is being formed when you bubble gas into the solution, the reaction is finished and you can filter out the brown goo.
> 
> *6. The crude salt, dissolved in boiling methanol, was added to chill acetone to form a crystalline product.*
> 
> The "crude salt" is the brown goo. Pour it into some boiling methanol under stirring. When all is dissolved, let chill down for a bit and then pour the mix into ice cold acetone. NOW you'll get the nice MDMA crystals.



DocXcould you please explain me more about the cilled acetone? would not be enough put the goo in saturated solution solvent, the wait to cristalize?
tnx!


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## 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...


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## 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


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## Mclssmxxl

IM BATMAN said:


> 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



IM BATMANI 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.


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## IM BATMAN

Mclssmxxl said:


> 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.



MclssmxxlTnx friend , i'll try for sure!


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## G.Patton

UnknownRadar said:


> For „NMF“ (its C2H5NO) I only can order this reagents „ACETAMID“
> 
> will it work too? @G.Patton
> 
> Summenformel: C2H5NO
> 
> Molare Masse: 59,07g/mol
> 
> CAS-Nummer: 60-35-5



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


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## RA!NER

William Dampier said:


> *Reaction scheme:*
> View attachment 1473
> 
> *Synthesis:*



William DampierHow many diethylether how many methanol how many aceton?


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## G.Patton

RA!NER said:


> diethylether



RA!NER2 x50 mL


RA!NER said:


> how many methanol


as small as possible to dissolve it


RA!NER said:


> how many aceton


approximately 1.5 volume of methanol


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## RA!NER

Thank you


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## ossi

William Dampier said:


> *Reaction scheme:*
> View attachment 1473
> 
> *Synthesis:*
> 1. Formic acid (3,66 g), NMF (7,6 g) and PMK (9.0 g) were refluxed at 150-170 *C for 7 h with additional formic acid (7,32 g) added periodically.
> 2. On cooling, a clear yellow solution of N-formyl-3,4-methylenedioxymethylamphetamine (N-formylMDMA) was obtained.
> 3. Concentrated hydrochloric acid (30 ml) was added to this solution, which was refluxed for a further 3 h.
> 4. The reaction mixture was made basic with sodium hydroxide, and the crude MDMA extracted into diethyl ether.
> 5. Next, the organic solvent was evaporated, the remaining residue was treated with hydrogen chloride gas to yield a gelatinous brown precipitate of impure MDMA hydrochloride.
> 6. The crude salt, dissolved in boiling methanol, was added to chill acetone to form a crystalline product.
> 7. This was recrystallized to yield fawn crystals with a melting point of 147 - 148 *C.



William Dampierplease please video


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## RA!NER

William Dampier said:


> View attachment 7030
> *Reaction scheme:*
> View attachment 1473​*Equipment and* *glassware**:*
> 
> 100 ml round bottom flask;​
> Retort stand and clamp for securing apparatus (optional);​
> Reflux condenser;​
> Heating plate;​
> Funnel;​
> Syringe or Pasteur pipette;​
> pH indicator papers;​
> Beakers (250 mL x2, 100 mL x4);​
> Vacuum source;​
> Laboratory scale (0.01-100 g is suitable);​
> Measuring cylinders 10 mL and 100 mL;​
> Water bath;​
> Glass rod and spatula;​
> Separatory funnel 0.5 L;​
> Laboratory grade thermometer (up to 200-250 °C); ​
> Buchner flask and funnel; ​
> Filter paper;​
> 
> *Reagents:*
> 
> Formic acid 10.98 g;​
> n-Methylformamide (NMF) 7.6 g;​
> MDP2P (PMK) 9.0 g;​
> Concentrated hydrochloric acid (HCl 36%) 30 ml;​
> Sodium hydroxide solution (NaOH 35%) ~10 ml;​
> Diethyl ether (or petroleum ether) ~150 ml;​
> Magnesium sulphate (MgSO4) ~15 g;​
> Methanol (MeOH) ~50 ml;​
> Acetone ~50 ml;​
> 
> *Synthesis:*
> *1.* Formic acid 3.66 g, n-methylformamide (NMF) 7.6 g and MDP2P (PMK) 9.0 g are placed into a 100 ml round bottom flask. Reflux condenser and thermometer are installed.
> *2.* The mixture is refluxed at 150-170 °C for 7 h with periodic formic acid 7.32 g additions.
> *3.* After that, the reaction mixture is cooled down to room temperature, a clear yellow solution of N-formyl-3,4-methylenedioxymethylamphetamine (N-formyl-MDMA) is obtained.
> *4.* Concentrated hydrochloric acid (HCl 36% 30 ml) is added to this solution. Than, reaction mixture is refluxed for additional 3 h.
> *5.* The reaction mixture is alkalized with several portions of sodium hydroxide solution (NaOH 35%) to 12 pH. Do not overheat reaction mixture.
> *6.* Crude MDMA free base is extracted from the alkaline solution with diethyl ether (or petroleum ether) 2 x 50 mL. Ether extract with MDMA free base is dried over MgSO4.
> *7.* After that, organic solvent is evaporated with a slight heating of warm water bath or with help of rotary evaporator with vacuum. MDMA free base oil is treated with hydrogen chloride gas and gelatinous brown precipitate of impure MDMA hydrochloride is obtained.
> *8. *The crude MDMA hydrochloride salt is dissolved in minimum volume of boiling methanol (MeOH), which is necessary to dissolve MDMA crude salt. Hot solution is poured into a beaker with chilled acetone, crystals are formed. This mixture is cooled down to a room temperature and vacuum filtered, crystals are washed with small amount of cold dry acetone and air dried (or dried in a vacuum chamber). Crystalline MDMA hydrochloride is obtained as the product.
> *9. *MDMA hydrochloride can be recrystallized one more time to yield fawn crystals with melting point 147 - 148 °C.​



William DampierGuys 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.


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## Curiousonion

RA!NER said:


> 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.



RA!NER"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?


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## RA!NER

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


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## Curiousonion

RA!NER said:


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



RA!NERWell 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.


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## RA!NER

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


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## Curiousonion

RA!NER said:


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



RA!NERWell 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.


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## RA!NER

Well thanks I will try


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## RA!NER

You me



Curiousonion said:


> 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.



Curiousonionan heating or distill or hcl Gas?


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## Curiousonion

RA!NER said:


> You me
> 
> an heating or distill or hcl Gas?



RA!NERNot 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.


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## G.Patton

Curiousonion said:


> 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.



CuriousonionAgree. 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.


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## RA!NER

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


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## Curiousonion

RA!NER said:


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



RA!NERUse acetone if you can't get ether then. Or ipa


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## RA!NER

I have ipa ok perfect


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## Curiousonion

Make sure you dry it


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## johnholding

Anyone had any issues with this method before i proceed to try??


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## Curiousonion

At what temperature do you reflux once you add the hcl?


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## G.Patton

Curiousonion said:


> At what temperature do you reflux once you add the hcl?



CuriousonionRead about Boiling point please. You have to reach this point and keep the reaction mixture for 3h. Also, there is written 150-170 °C.


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## Curiousonion

Yes but boiling point of formic acid boiling point is 100c and thats for the first step.
So ill assume second step is 150-170c as well.



G.Patton said:


> Read about Boiling point please. You have to reach this point and keep the reaction mixture for 3h. Also, there is written 150-170 °C.



G.Patton


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## T0R

G.Patton said:


> Read about Boiling point please. You have to reach this point and keep the reaction mixture for 3h. Also, there is written 150-170 °C.



G.Patton
unpossible with HCI 
but in this step you dont over heat the flask becouse other wise you get black teer . Check you boiling point by add a small stone in your flask. My guess temp goes max 75°c

only with the use off vacuum, you can raise temp


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## Curiousonion

Ah ok, so you recommend to reflux it at 75c? 
I don't think it needs such a high temperature with hcl.


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## G.Patton

Curiousonion said:


> Ah ok, so you recommend to reflux it at 75c?
> I don't think it needs such a high temperature with hcl.



CuriousonionYou have to reach boiling. Also, @Saul is right about boiling chips.


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## Curiousonion

G.Patton said:


> You have to reach boiling. Also, @Saul is right about boiling chips.



G.PattonI usually use stirring when boiling my reactions. I find it's more efficient than boiling stones


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## G.Patton

Curiousonion said:


> I usually use stirring when boiling my reactions. I find it's more efficient than boiling stones



CuriousonionYour stirring bar makes boiling centers like boiling chips.


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## johnholding

*Synthesis:*
1. Formic acid (3,66 g), NMF (7,6 g) and PMK (9.0 g) were refluxed at 150-170 *C for 7 h with additional formic acid (7,32 g) added periodically.
2. On cooling, a clear yellow solution of N-formyl-3,4-methylenedioxymethylamphetamine (N-formylMDMA) was obtained.
3. Concentrated hydrochloric acid (30 ml) was added to this solution, which was refluxed for a further 3 h.

What temperature do i reflux this at? 

4. The reaction mixture was made basic with sodium hydroxide, and the crude MDMA extracted into diethyl ether.
5. After the volume of the organic solvent was decreased, the remaining residue was treated with hydrogen chloride gas to yield a gelatinous brown precipitate of impure MDMA hydrochloride.
6. The crude salt, dissolved in boiling methanol, was added to chill acetone to form a crystalline product.
7. This was recrystallized to yield fawn crystals with a melting point of 147 - 148 *C. 

Also will there be a video on this method?


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## G.Patton

johnholding said:


> What temperature do i reflux this at?



johnholdingMaintain the temperature when the boiling starts. It named boiling temperature.


johnholding said:


> Also will there be a video on this method?


probably yes


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## ossi

William Dampier said:


> MDP2P (PMK)



William Dampiercan i have CAS please?


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## ossi

William Dampier said:


> View attachment 7030
> *Reaction scheme:*
> View attachment 1473​*Equipment and* *glassware**:*
> 
> 100 ml round bottom flask;​
> Retort stand and clamp for securing apparatus (optional);​
> Reflux condenser;​
> Heating plate;​
> Funnel;​
> Syringe or Pasteur pipette;​
> pH indicator papers;​
> Beakers (250 mL x2, 100 mL x4);​
> Vacuum source;​
> Laboratory scale (0.01-100 g is suitable);​
> Measuring cylinders 10 mL and 100 mL;​
> Water bath;​
> Glass rod and spatula;​
> Separatory funnel 0.5 L;​
> Laboratory grade thermometer (up to 200-250 °C); ​
> Buchner flask and funnel; ​
> Filter paper;​
> 
> *Reagents:*
> 
> Formic acid 10.98 g;​
> n-Methylformamide (NMF) 7.6 g;​
> MDP2P (PMK) 9.0 g;​
> Concentrated hydrochloric acid (HCl 36%) 30 ml;​
> Sodium hydroxide solution (NaOH 35%) ~10 ml;​
> Diethyl ether (or petroleum ether) ~150 ml;​
> Magnesium sulphate (MgSO4) ~15 g;​
> Methanol (MeOH) ~50 ml;​
> Acetone ~50 ml;​
> 
> *Synthesis:*
> *1.* Formic acid 3.66 g, n-methylformamide (NMF) 7.6 g and MDP2P (PMK) 9.0 g are placed into a 100 ml round bottom flask. Reflux condenser and thermometer are installed.
> *2.* The mixture is refluxed at 150-170 °C for 7 h with periodic formic acid 7.32 g additions.
> *3.* After that, the reaction mixture is cooled down to room temperature, a clear yellow solution of N-formyl-3,4-methylenedioxymethylamphetamine (N-formyl-MDMA) is obtained.
> *4.* Concentrated hydrochloric acid (HCl 36% 30 ml) is added to this solution. Than, reaction mixture is refluxed for additional 3 h.
> *5.* The reaction mixture is alkalized with several portions of sodium hydroxide solution (NaOH 35%) to 12 pH. Do not overheat reaction mixture.
> *6.* Crude MDMA free base is extracted from the alkaline solution with diethyl ether (or petroleum ether) 2 x 50 mL. Ether extract with MDMA free base is dried over MgSO4.
> *7.* After that, organic solvent is evaporated with a slight heating of warm water bath or with help of rotary evaporator with vacuum. MDMA free base oil is treated with hydrogen chloride gas and gelatinous brown precipitate of impure MDMA hydrochloride is obtained.
> *8. *The crude MDMA hydrochloride salt is dissolved in minimum volume of boiling methanol (MeOH), which is necessary to dissolve MDMA crude salt. Hot solution is poured into a beaker with chilled acetone, crystals are formed. This mixture is cooled down to a room temperature and vacuum filtered, crystals are washed with small amount of cold dry acetone and air dried (or dried in a vacuum chamber). Crystalline MDMA hydrochloride is obtained as the product.
> *9. *MDMA hydrochloride can be recrystallized one more time to yield fawn crystals with melting point 147 - 148 °C.​



William Dampierplease can write someone big scale?


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## Curiousonion

Did you try it first scale to see if you can do the rxn first?



ossi said:


> please can write someone big scale?



ossi


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## ossi

Curiousonion said:


> Did you try it first scale to see if you can do the rxn first?



Curiousonionofc i try first this scale


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## Curiousonion

ossi said:


> ofc i try first this scale



ossiAnd how did it go?


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## ossi

Curiousonion said:


> And how did it go?



Curiousonionsorry, my english is not so good, german better. i mean i want try first same as here written, still waiting reagents.
but i'm confident


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## Curiousonion

I tried this conversion recently, did the nmf with formic acid and pmk reflux for 7 hours. Cooled it down then added the 37% hcl, no reaction since it is acid to acid.
Then started refluxing it, as soon as it went over 84c the mixture started to turn into a brown sludge. 
I think its wiser to reflux the hcl at around 60c. 

Any one has any experience with this reaction and can help?

Thanks


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## ossi

Curiousonion said:


> I tried this conversion recently, did the nmf with formic acid and pmk reflux for 7 hours. Cooled it down then added the 37% hcl, no reaction since it is acid to acid.
> Then started refluxing it, as soon as it went over 84c the mixture started to turn into a brown sludge.
> I think its wiser to reflux the hcl at around 60c.
> 
> Any one has any experience with this reaction and can help?
> 
> Thanks



Curiousonionhi, you solve this problem meanwhile?


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## Curiousonion

ossi said:


> hi, you solve this problem meanwhile?



ossi
No, not yet.
Trying the reaction again today but going at 45-55c for 6 hours instead of higher temp for 3 hours. 
So far it looks better than the previous reaction, it did not turn into tar although it was not a clear yellow after the 7 hour reflux with formic acid as described by op.


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## ossi

Curiousonion said:


> No, not yet.
> Trying the reaction again today but going at 45-55c for 6 hours instead of higher temp for 3 hours.
> So far it looks better than the previous reaction, it did not turn into tar although it was not a clear yellow after the 7 hour reflux with formic acid as described by op.



Curiousonionwould be great if you update here 
good luck


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## Curiousonion

ossi said:


> would be great if you update here
> good luck



ossiOn second try I refluxed it with the hcl for 6 hours. It stayed a brown liquid.
I added naoh solution to bring ph up (takes a lot of naoh in order to do that).
Seperated with dcm after, separation has a lot of salt residue in it.
Evaporated the dcm and got left with a brown syropy liquid. 
I added some hcl to it to bring ph down and now attempting to crystalize it. (unsuccessfully so far)


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## ossi

Curiousonion said:


> On second try I refluxed it with the hcl for 6 hours. It stayed a brown liquid.
> I added naoh solution to bring ph up (takes a lot of naoh in order to do that).
> Seperated with dcm after, separation has a lot of salt residue in it.
> Evaporated the dcm and got left with a brown syropy liquid.
> I added some hcl to it to bring ph down and now attempting to crystalize it. (unsuccessfully so far)



CuriousonionI'm very curious what the experts will say about this
@William Dampier 
@G.Patton


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## Curiousonion

Honestly it's not the best method. 
There is another rxn writeup on this thread where they use 180 to start on an industrial scale. They distill the formic acid they don't reflux it and I understand why, too much acid to neutralize at the end.
But now I'm having trouble crystalizing it.
I added hcl to the goo then added hot methanol and then poured it into cold acetone and placed it in a freezer. But I doubtvl that would work


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## ossi

Curiousonion said:


> poured it into cold acetone



Curiousonionin this point no crystallization?


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## Curiousonion

ossi said:


> in this point no crystallization?



ossiNone what so ever. 
Could be due to water residue or dcm residue. 
Next I'll try to make some acidic water and see if the mdma freebase gets pulled into it from the dcm and then boil the water off.


----------

