# MDP2P to MDMA without Methylamin (copied from the internet)



## Jesse_Pinkman_ (Sep 25, 2022)

Who Needs Methylamine Anyway?
By Ritter, edited by the Professor, Dedicated to Eleusis
Published in Total Synthesis II by Strike

The following procedure may prove to be one of the largest advances in the field of MDMA chemistry since the perfection and dissemination of the Wacker oxidation procedure for producing MDP2P. This reaction is based on a published process that somehow has escaped discovery by underground chemistry until now. Methylamine is no longer a stumbling block in the aluminum amalgam reductive alkylation method of producing MDMA as this procedure produces this impossible to obtain and fickle to make material, in situ, during the reductive alkylation of MDP2P to MDMA from very common nitromethane. Nitromethane when subjected to the simplest of reductions forms methylamine, so why not make methylamine at the same time MDMA is being produced instead of going through the hassle of making it separately?

Nitromethane is a very common material. Just go down to your local drag strip and pick up a gallon or two for doping your high performance car’s fuel. It’s also available up to 40% pure in RC model fuels. Simply fractionally distill the nitromethane (bp 101°C) out of the model fuel mixture and you’re ready to go. If methanol is present in the fuel formulation, some will azeotropically distill over with the nitromethane lowering its boiling point slightly, but this does not present a problem.

So, how does this whole thing work? It’s as simple as it sounds. An alcoholic solution of nitromethane and MDP2P is dripped into a mass of amalgamated aluminum immersed in alcohol first reducing the nitromethane to methylamine, allowing the Schiff base of the amine and ketone to form which is further reduced to the desired MDMA 
Set up a 2 liter two or three-neck flask with an addition funnel and a reflux condenser and provide with a heat source. Not much heat is needed here so anything from a water bath on a buffet range to a heating mantle is fine. Stuff 55 grams of one-inch squares of aluminum foil into the flask. An important topic must be addressed here which has been formerly neglected to a confusing degree – the proper type and thickness of the foil. The problem with aluminum amalgam reductions is that their reaction rate is dependent on three major factors, and depending on how you play these factors you may either have a complete failure or an explosion, or better yet if you follow this advice, a perfect yield! These factors are the mentioned foil type, the degree of amalgamation allowed by HgCl2 solution before ketone and amine are reacted, and finally, the temp the reaction runs at. Thick foil tends to react slowly at a low temp and very thin foil, such as generic food grade aluminum foil, tends to react so fast and exothermically you can literally shit your pants! The aluminum, which produced the best results, is widely available to the industrial biological community in the form of 4" x 4" sheets .04mm thick neatly separated from each other with a sheet of tissue paper. It is used for sealing flasks and the like before they are autoclaved. For those of you who can’t get this, don’t worry. Heavy Duty Reynolds Wrap will work fine, only a more careful eye must be kept on the reaction rate. Others have reported success using cut up pie tins. The main idea is don’t use real thin foil.

Fill the separatory funnel with 50 grams of MDP2P and 50 grams or 39ml nitromethane dissolved in 200ml methanol. In another 1 liter vessel, add 1.5g HgCl2 (mercuric chloride) to a liter of methanol and allow all solids to dissolve. Very carefully (HgCl2 is deadly poisonous!) pour the methanolic solution of HgCl2 onto the aluminum foil pieces in the flask and stand back and watch the magic begin. If all the foil isn’t covered by the methanol just add more until it is. In a few minutes effervescence will begin and the reaction may be started. After about 5-10 minutes the bubbling should be sufficient and you may start adding the methanolic mixture of nitromethane and MDP2P drop by drop from the separatory funnel. As time progresses the reaction may heat up to the point of boiling and refluxing of the alcohol will occur. This is no problem as the 65°C boiling point of methanol is perfect for this reaction (I know many disagree, but dream about this and you’ll see!) The addition should take roughly one hour and the mixture should be allowed to react for at least 4-6 hours after or until all pieces of aluminum are reacted into gray suspension. Temperature control needs to be addressed here. If the reaction proceeds under ideal conditions, it will run exactly as described above. If less than ideal and more commonly, the reaction will start to slow down halfway through requiring external heating to maintain a good reaction rate. If the Greater Powers are really against you, an addition of another gram of HgCl2 in methanol solution to the mix will kick it back in.
Now the easy part – isolating your product. One of the most attractive features of this new synthesis is that the standard Al/(Hg) amination mixture must be tediously filtered to separate the product from the spent aluminum hydroxide sludge at this point. The following remedies this most frustrating step and will probably give many a new outlook on the potential of the Al/(Hg) reduction.

Mix up about 1.5 or 2 liters of 35% NaOH solution and allow to cool. Slowly add the gray aluminum gook produced in the first reaction to the NaOH solution and pour into a large separatory funnel. Two distinct layers will appear after sitting for maybe an hour, the top being a reddish alcoholic solution of product and the bottom garbage NaOH/Al(OH)3. Simply separate off the garbage bottom layer and discard. Don’t worry, there’s no product tied up in it, and remember that no filtration is needed anywhere in this recovery process compared to other synths out there! Take the top layer and evaporate off the methanol to give an amazing yield of impure amine and a little bit of water. Unscrupulous souls not worth their weight in shit can take this product and crystallize it directly but there is a lurking deadly poison in it at this point – solvated mercury salts! These can be easily removed by dissolving the crude product in about a liter of toluene and washing it with several portions of water in a separatory funnel and finally with a saturated NaCl solution. Dry the toluene with about 50g anhydrous MgSO4 made by heating drug store epsom salts in the oven at 400 degrees Fahrenheit for an hour, cooling then powdering. After sitting for an hour or until the toluene is no longer cloudy, chill the dried toluene solution of freebase in the freezer and bubble away with HCl gas to produce beautifully pure MDMA hydrochloride crystals. If they are a little discolored they can be cleaned up with an acetone rinse to pristine purity with no mercury contamination!


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## Jesse_Pinkman_

Also found this one:

Pmk 
I had some MDP-2-P lying around in the freezer that I'd made in late November, and I really wanted to get rid of it for two reasons: I didn't want it go bad, and I really didn't like having a List I precursor sitting in my freezer. I'd always had some problems doing the Al/Hg with methylamine so I decided to give the nitromethane Al/Hg a whirl. Methyl Man seemed proud of his variation, recently posted on the Hive, so I chose his parameters for the reaction.

I have to begin by saying that this is a killer reaction. Methyl Man's pride is totally justified. My yields were awesome and the purity was excellent. I did the whole reaction, with crystallization, in the span of an evening. The reduction ran hot but was completely under control, easily stirred, fast, and simple to work up.

I set up a two-liter flat-bottom three-neck flask, and plugged one of the necks. I arranged to have an ordinary condenser in the center hole. The apparatus was placed on my stirrer/hotplate.

I started cutting Reynolds Heavy Duty aluminum foil into about 1" squares, to make a total of 27.5g. You just have no idea how much foil is 27.5g until you actually start cutting it up. It must have taken nearly half an hour, and it seriously dulled my scissors. I put 5g batches into a small Braun coffee grinder and ground the foil for 8-10 seconds. The foil doesn't really get "ground", but as Methyl Man says, it gets all balled up into little globs. This worked amazingly well. It may sound weird to put your foil in a coffee grinder, but this is without question a breakthrough in the preparation of aluminum for the Al/Hg.



Figure 1: 5g of foil in 1" squares
Figure 2: 5g of foil, after 8-10 seconds of grinding in a Braun coffee grinder


Figure 3: Closeup of foil balls
Figure 4: 27.5g foil in a 2000 mL flat-bottom flask
The foil balls were dumped in the flask.

Next, 400mg of HgCl2 was dissolved in 750 mL of lab grade MeOH. While this was being done, 25g of MDP-2-P and 20g of ACS nitromethane were mixed in a dropping funnel with a bit (probably about 25 mL) of MeOH. The MDP-2-P was three months old and had been stored in the freezer. It had been distilled originally, still smelled good and was a medium-light green color. The dropping funnel was put on a side neck on the flask.


Figure 5: Apparatus
When the MeOH was ready (all HgCl2 dissolved), it was also dumped in the flask and the condenser was put in place. As Methyl Man instructed, it was stirred for 5-10 seconds every minute or so. In less than 10 minutes, faint bubbling was visible, the solution was gray, and the aluminum was distinctly less shiny. Some pieces had started to float.


Figure 6: Amalgamation complete
Ice water was started flowing through the condenser. About 4 pounds of ice in 2.5 gallons of water was used, in a 5 gallon paint bucket.

The valve on the dropping funnel was opened so that the mix started dripping at around one drop per second. About every minute, I turned on the stirrer for about 5 seconds. After just a few minutes, the flask started to heat up, and I started stirring continuously. At this point the mix had a very distinct steel blue-gray color, like Methyl Man describes.



Figure 7: Reaction starting, t+7 minutes
Figure 8: Approaching reflux temp., t+8 minutes
Eventually the reaction heated itself up to an impressive reflux, and MeOH was flowing nearly continuously from the condenser. I had to adjust the drip speed from time to time (one per second was a little too slow) and I finished the addition after 42 minutes. During the peak of the reaction, I watched what was going on very closely, but I really didn't need to do anything at all except make sure that the addition was going at a rate that would make the whole thing take 40-45 minutes. Everything else took care of itself.


Figure 9: Reaction going full blast, t+15 minutes
By the time I had a few milliliters of MDP-2-P mix left to go, the reaction was already starting to slow down, though there were still some small aluminum flakes visible. This is exactly in line with Methyl Man's instructions. The mix was starting to get very viscous, so I added another 50-75 mL of MeOH down the condenser which greatly improved things. I then left for about an hour to let the reaction finish itself.

When I got back things had cooled considerably and the mix was mostly an amorphous gray with just the tiniest flecks of white mixed in. I mixed 700 mL of water and 262g of NaOH in a beaker. While this was cooling, I dumped the contents of the reaction flask into a 4000 mL beaker. A bit more (maybe 50 mL) MeOH in the reaction flask easily loosened the remaining sludge, and this was dumped into the beaker too. Then the NaOH solution was poured into the 4000 mL beaker with the sludge.



Figure 10: Sludge in the beaker
Figure 11: Sludge after NaOH addition and a little stirring
A 3" stirbar was put in the beaker and it was thoroughly stirred. The formerly gray sludge turned darker, and the NaOH started reacting with the remaining aluminum, making a foamy, smelly mess in the beaker. It warmed up slightly but not appreciably. This was left to stir slowly for about an hour, at which time almost all the bubbling was done and the foaming had decreased.

I do not own a gigantic sep funnel, so I decided to extract the mix directly in the beaker. This actually works really well and may be easier than dealing with a sep funnel. 500 mL of toluene was dumped in the beaker, and the stirrer was turned on very high for several minutes. This mixed the two phases well. Over the next 15 minutes or so, the toluene separated out to the top.



Figure 12: Bubbling as NaOH reacts with remaining aluminum
Figure 13: Toluene after mixing, mostly done separating.
I was worried, because the toluene had virtually no color to it. I would expect there to be some remaining MDP-2-P with its slight color, or for some reaction impurities to give a color too. But this was slightly milky white. Toluene is kina hard for me to get, so next time I plan to try xylene instead. I suspect this will work fine.

Most of the toluene was poured off the top. About 100 mL was left, because it became difficult to get the toluene off without some of the water/sludge layer also pouring out. Another 250 mL of toluene was dumped in the beaker and thoroughly mixed. This next extraction was also poured off, this time with a bit of the sludge layer, and put in the sep funnel. There was probably no more than about 15 mL of toluene left floating on the sludge in the beaker when I was done. Now it was easy to drain off the sludge layer in the sep funnel, leaving only toluene. The first toluene extraction was then added to the sep funnel.



Figure 14: About to drain off the very last bit of sludge-water
Figure 15: Washing. Both the toluene and wash are very clean, and the interface between layers is barely visible 3/4 of the way down the picture.
The toluene was washed twice with saturated sodium bicarbonate, once with saturated NaCl, and once with water. All of the washes were quite clean, and the toluene was looking even cleaner than before.

The toluene was drained into a washed, acetone-rinsed, thoroughly dried beaker with about 35g anhydrous MgSO4. This was left for about 25 minutes and stirred with a spatula two or three times. It was then filtered into a new beaker (also super dry), and the MgSO4 in the filter washed with a little new toluene.

A standard NaCl/H2SO4 generator for HCl gas was set up, with a fractionating column packed with CaCl2 (Damp-Rid from Home Depot) as a drying tube. A gas dispersion tube with a porous glass disc was attached to the drying tube, and the H2SO4 was started dripping.

Gas began to come out of the dispersion tube, which I immersed in the toluene filtrate. Absolutely nothing had happened after several minutes and I was convinced I had totally fucked up. Then a wisp here and there of white material started to appear, and within 30 seconds there were giant clouds of puffy MDMA HCl cascading out of solution. I nearly shit my pants.



Figure 16: Crystals forming as the HCl exits the gas dispersion tube.
Figure 17: Getting near the end of this gassing run. The crystals are settling, and have formed a thick layer at the bottom of the beaker.
I would recommend against using a gas dispersion tube, since it seems to clog up with crystals and generate serious backpressure in the HCl generator. At one point, a glass stopper popped right off the apparatus, there was so much pressure. Just use a glass tube to get your HCl into the toluene.

The solution was so cloudy that I couldn't tell if any more crystals were precipitating, so I decided to stop. The beaker was covered and put in the freezer for half an hour. When cold, it was filtered with vacuum in a Buchner, then dried on a mirror under a light bulb (for heat) and weighed. There was a total of 8.26 g.

Then I set up to gas the toluene again. And lo and behold there was another massive precipitation of crystals. The toluene was chilled and filtered and the filtrate dried, yielding another 4.72 g!

Set up to gas again... it just keeps on coming. I give the crystals some time to settle, and now there really doesn't seem to be any more coming out of solution. Chill, filter and dry. This time there was 6.61 g more!

Even though the crystals had a slight (and very pleasing) root beer odor, I decided against recrystallizing because the crystals were blindingly bright white and obviously of good purity.



Figure 18: A Buchner funnel tightly packed with crystals
Figure 19: 8.26 grams of MDMA HCl, chopped up and drying on a mirror
Total yield: 19.6 grams of MDMA HCl - from 25 grams of ketone !!

Bioassay: Unqualified success.

I have to say that Methyl Man has scored a serious winner with this procedure, especially with the management of the amalgam. He's figured out how to make it easy to stir, how to make it run at the right rate, and how to work it up way more easily than I've ever seen.

And you don't even need to make methylamine!

This, in conjunction with Bright Star's writeup of the ketone synthesis and purification, makes for the most straightforward MDMA synthesis the Hive has ever seen.

Reference: Methyl Man's Reductive Amination
The toluene was washed twice with saturated sodium bicarbonate, once with saturated NaCl, and once with water. All of the washes were quite clean, and the toluene was looking even cleaner than before.

The toluene was drained into a washed, acetone-rinsed, thoroughly dried beaker with about 35g anhydrous MgSO4. This was left for about 25 minutes and stirred with a spatula two or three times. It was then filtered into a new beaker (also super dry), and the MgSO4 in the filter washed with a little new toluene.

A standard NaCl/H2SO4 generator for HCl gas was set up, with a fractionating column packed with CaCl2 (Damp-Rid from Home Depot) as a drying tube. A gas dispersion tube with a porous glass disc was attached to the drying tube, and the H2SO4 was started dripping.

Gas began to come out of the dispersion tube, which I immersed in the toluene filtrate. Absolutely nothing had happened after several minutes and I was convinced I had totally fucked up. Then a wisp here and there of white material started to appear, and within 30 seconds there were giant clouds of puffy MDMA HCl cascading out of solution. I nearly shit my pants.
I would recommend against using a gas dispersion tube, since it seems to clog up with crystals and generate serious backpressure in the HCl generator. At one point, a glass stopper popped right off the apparatus, there was so much pressure. Just use a glass tube to get your HCl into the toluene.

The solution was so cloudy that I couldn't tell if any more crystals were precipitating, so I decided to stop. The beaker was covered and put in the freezer for half an hour. When cold, it was filtered with vacuum in a Buchner, then dried on a mirror under a light bulb (for heat) and weighed. There was a total of 8.26 g.

Then I set up to gas the toluene again. And lo and behold there was another massive precipitation of crystals. The toluene was chilled and filtered and the filtrate dried, yielding another 4.72 g!

Set up to gas again... it just keeps on coming. I give the crystals some time to settle, and now there really doesn't seem to be any more coming out of solution. Chill, filter and dry. This time there was 6.61 g more!

Even though the crystals had a slight (and very pleasing) root beer odor, I decided against recrystallizing because the crystals were blindingly bright white and obviously of good purity.

•HgCl2 
•MeOH 
•ACS nitromethane 
•NaOH 
•Beaker 
•Dropping funnel 125ml 
•Toluene 
•Xylene 
•Sep funnel 
•Saturated sodium bicarbonate 
•Saturated NaCl
•Anhydrous MgSO4 
•Spatula 
•Reflux condenser 
•Heavy Duty Reynolds Wrap


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## Fenster

I'm surprised this has not got more attention. 

I see so many meth synth teks that require Methylamine yet no one has suggested making it in situ. via addition reduction of nitromethane using the same amalgam your reducing your ketone with. Sure if this works for MDP2P then it will work with P2P. I don't know about you, but RC fuel is a lot less fucking around then making a Methylamine solution an adding it in.


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## TotalSynthesis

It is published in the Fester's book, so i guess it is quite famous but the downside of it is that one has to go via al/hg.

RC fuels better should be distilled before usage because they mightr contain up to 10% oil! When distilling nitromethane, please dont use a electric vacuum pump but an aspirator to avoid any danger of explosions caused by a short or anything like that !!


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## Fenster

So the suggestion is to go for NaBH4 but good luck getting that OTC in some parts of the world  

Nitromethane can be found at 99% concentrations, all of the videos on this site recommend you make Methylamine and add it, none of them follow this method and I wonder if it's habit or it's actually down to something more pragmatic.


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## TotalSynthesis

NaBH4 is not the only alternative to al/hg.
there are many.

But in general you're ofcourse right, it might be easier


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## cubesquare

Jesse_Pinkman_ said:


> Also found this one:
> 
> Pmk
> I had some MDP-2-P lying around in the freezer that I'd made in late November, and I really wanted to get rid of it for two reasons: I didn't want it go bad, and I really didn't like having a List I precursor sitting in my freezer. I'd always had some problems doing the Al/Hg with methylamine so I decided to give the nitromethane Al/Hg a whirl. Methyl Man seemed proud of his variation, recently posted on the Hive, so I chose his parameters for the reaction.
> ...



Jesse_Pinkman_I would love to see this with all the actual images...


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## Fenster

cubesquare said:


> I would love to see this with all the actual images...



cubesquareIt's available, with a little bit of searching


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## Fenster

What I want to see is adaptation of this procedure to apply to P2P. To remove the need for pre production of Methylamine on under 100g ketone reductions.


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