Mephedrone (4-MMC) Synthesis [2B4M, Ethyl Acetate, Methylamine HCl]

[William Dampier]

As Hanna520 wrote in the another thread, it is better to prepare alc. methylamine for this synthesis. You will get fewer problems associated with the hydrolysis of ethyl acetate. You can use triethylamine, ethanol or methanol, or THF. Get a solution of gas and a precipitate of salts without water. It is easy to separate by decanting and you can start your synthesis more successfully. For small quantities this is usually not a problem, but if you want to synthesize several kg at a time it will be significantly different.

 

[Ranbir Singh]

Hellow sir can I boiling after layer saperate than acidification
Any problem

 

[Dr. MMX]

Yes this is very good reagent, to ensure maximum precise, but most important is 2b4m, rest matters less

 

[zetvasa9]

Hello, we have synthesized this method 3 times but we do not get more than 30% yield, what could be the problem? We follow the technology 1 in 1 as described in the guide

 

[handle]

I'm next going to try to extend reaction time by 1 hour from 4 hours up too over night. with light heating 28-33c after the forth hour, as thats when my reaction starts to cool down naturally.,

 

[SpaceRocket]

I did 2 batches yesterday. I let one batch react for 2 hours at 30 degrees Celsius. I let the other batch react for 45 minutes, but then at a high temperature. The maximum temperature was 54.5 degrees Celsius. With these batches, much more HCl was added at the end than with the 2 batches before. This is usually a sign that there will be more end product.

 

[handle]

we could try an alternate solvent like DMSO rather than Ethyl Acetate, maybe? IDK sorry.

 

[nimrod313]

WWork with dcm no more 38⁰

 

[handle]

I can never get it to 5.5 !! its always hangs around 7 - 8, then sometimes jumps straight up to 4...
So Annoying... by that time i think it has already mostly all come out of solution anyway, is there any point adding more HCl if solution has already precipitated? at 7 or 8?

 

[nimrod313]

Better make it 5-6 if you got salts dilute it for better stirr

 

[norivotset69]

are there any major differences when using 40% aq methylamine? 70g of it? does the reaction work same, duration etc?

 

[Dr. MMX]

Precisely, for each mole of 2b4m is 2 moles of methylamine.

In the practice, yes you can do use about 135 ml of methylamine for 100g of 2b4m for the reaction.
You do not need to steps regarding usage of NaOH used to generate methylamine gas.

 

[norivotset69]

The reaction was takin about 8 hours (i still dont know how long should it last) and the color was dark dark turquise (visible through strong light). Changed to brown after rinsing with sodium bicarbonate. After rinsing I was left with 50ml of solvent (used 250 at the beggining). Is that solvent emulsified? I waited few minutes for every layer separation. Also liquid is then very dark color and when adding acid it doesnt change white but more of a yellowish milk coffee.

 

[zetvasa9]

Hello, we have synthesized this method 3 times but we do not get more than 30% yield, what could be the problem? We follow the technology 1 in 1 as described in the guide. But the product comes out very good quality

 

[nimrod313]

Work with other solvent

 

[Alchemistfromthahood]

The last time I made 4 mmc, I used HCl gas instead of hydrochloric acid.
The result was better.
Perhaps it's the water, as some of the salt dissolves during precipitation. The experts among us can certainly provide better information on this.just wanted to try this way

 

[Russian lab assistant]

Hi, how did you use HCI gas? Can you tell me more?

 

[Alchemistfromthahood]

Hello
i used the instructions from this article

Dry HCl gas from muriatic and sulfuric acids conc.

Dripping an affordable muriatic acid (HCl aq 31%) over concentrated sulfuric acid (H2SO4) is one of the best methods for producing a dry gaseous HCl, if it is necessary to quickly scaling. The reaction rate and temperature is easily controlled. Capacities are easily and quickly cleaned, and if...

bbgate.com

the tubes should be teflon because other materials will dissolve
tube inside the freebase solution and you can start
it takes a while till you get the right settings for your setup but when you have it works great and safety

 

[Alchemistfromthahood]

Read this article and you have everything you have to know for this operation

 

[G.Patton]

Read more here https://safrole.com/knowledge-base/how-to-make-dry-hcl-gas/

 

[Alchemistfromthahood]

nice that you share it
thx

 

[lucas147]

Hello. My question is, if I use methylamine hcl, will the effect be the same as using methylamine 40%? or different..??

 

[G.Patton]

Hello, probably the same. Effects of 4-mmc depends on its isomers' composition.

 

[Alchemistfromthahood]

why do you take this solvent ratio of 2b4m and ethylacetate ? mostly I use a ratio of 100gr 2b4m and 200ml ethylacetat
is there a special reason you ratio ?

 

[TayRonz]

Can 2b4m be replaced by 2i4m for this reaction?
In case there's only access to MeNH2*HCl and not to the 40% solution. (Because in the rest of the guides I've seen posted here, 40% Methylamine solution is used and not the salt form)

 

[Dr. MMX]

I used more amount of solvent to make more quick reaction and to not get such such big temperature, it can be used with different proportions but I think minimum is 350-400 ml.

The method was only in the case when the aq40% is not aviable or for some reason it not result good synthesis. Method is not scalable very much, it will rinse a lot of problems when scaled up but its ok for this scale.

If somebody recieve smaller yield there can be a lot of reasons, based on the purity of regents used, the techniques performed.

The 2i4m probably could be used but I did not test it.

If you do have bad yield or your reactoin turns out not clean - please do remember that using methylamine hcl rather than aq results more impurities, as well the alcohol with metylamine. The reaction must be performed ASAP with no futher delays until acidificatoin. Longer it takes worse result will be.

Regards.

 

[Alchemistfromthahood]

I replaced the aqueous solution with hydrochloride because the smell is unbearable and everything smells of this chemical. Why do you think the synthesis isn't scalable? I've processed up to 5 kg of the precursor using your method and always had a yield between 55-60%. Aside from the fact that you do a bit of extra filtering, this route is very convenient in terms of handling.

 

[Alchemistfromthahood]

What I've noticed is that the longer the free base is left unacidified, the darker the color becomes. The free base starts off a beautiful yellow with a certain color density, then changes to green or dark green. However, this problem can be easily managed with a few optimizations in the workflow.