Mephedrone (4-MMC) synthesis from haloketone in ethyl acetate. 1-10 kg Scale.

[DavidNichols]

Ethyl Acetate (EA) is hydrolyzed by methylamine and gives ethanol and methylacetamide. Oxidization of 4-mmc freebase into acetate is also possible.

https://www.journal.csj.jp/doi/10.1246/bcsj.39.1837

Why performing the distillation of cheap EA, jeopardizing your valuable freebase if you can use easy-to-make HCL in EA and distill after that?

 

[Chemix-Express]

Having a pure 4MMC base in Toluene, can I add an equal volume of ethyl acetate and desalt with hydrochloric acid to PH 5.5 without any problem?

I have recently started doing this as I have ethyl acetate much cheaper than Acetone.

Will this negatively affect the yield or quality of the product?

 

[DavidNichols]

Yes, EA is a perfect solvent for water bonding if cant get IPA-HCL or EA-HCL. The losses from 4MMC-HCL dissolved in anhydrous EA are minuscule.

 

[Chemix-Express]

He is aware of this. Everyone recommends DCM. Unfortunately there, at 40 degrees C and a 2h response, it is necessary to use a reflux cooler, which with my volumes and workspace is not an option.

 

[DavidNichols]

40 degrees are not possible without extended amount of water in amination reaction. 38-39 at best. 2 hours is also a nonsense. You will end with high amount of pirazines, 4-MEC (in case of excessive amount of methylamine) and possible iso-mephedrone (havent been yet confirmed by experiments).

 

[w2x3f5]

at room temperature, the reaction proceeds for two hours with stirring. did you check on tсl? and why 4-mec (n-ethylcatinon)???

 

[w2x3f5]

del

 

[DavidNichols]

Right and valid correction. Made a mistake, meant N,N-Dimethyl Methcatinone. Any primary amine turns into secondary if there is enough time, energy and source. Reductive amination has the similar issue. Check MDDM contamination in MDMA clandestine synthesis. Overheating and wrong reaction times are causes of that.

 

[DavidNichols]

Addition to 4-MEC formation under extended reaction time under reflux in alkaline environment:

 

[w2x3f5]

Again, a mistake, there is an admixture of dimethylamine in methylamine (standard), because of this. This admixture of dimethylamine is always present in methylamine.

 

[w2x3f5]

In the document, I did not see anything other than the reaction of amine with formaldehyde (which in our case does not exist and there is nothing to restore even in the reaction). The document has nothing to do with the admixture of dimethylcathinone, or I didn’t see it, then if it’s not difficult for you, write where to look for the document.

 

[DavidNichols]

You can use DCE and get same timings as with DCM but without boiling.

 

[UWe9o12jkied91d]

Any idea if sodium hypochloride + alkaline metal salt of bromine will work for the bromination here? @William Dampier @G.Patton ?

 

[w2x3f5]

In hypochlorite there is an admixture of sodium hydroxide and it is quite significant, hypochlorite is not very stable and decomposes quickly during storage, especially concentrated solutions.
more better NaBr+NaBrO3+H2SO4

 

[G.Patton]

I don't think that it is good idea.

 

[DavidNichols]

Yes, any hypochlorite + bromide + strong acid (Cl or SO4). Any chlorate is will work too, but with less chlorine gas.

 

[w2x3f5]

Hypochlorite is stabilized with alkali and there is a significant amount of it, in addition, it will have to be titrated, since hypochlorite is relatively quickly destroyed during storage. The first thing that will bind alkali is hydrogen bromide, and only then sulfuric acid, as it seems to me. They took a very inconvenient oxidizing agent.

 

[madmoney69]

Is this is the most practical mephedrone synthesis when doing it on 100kg scale?

 

[$!$]

The best way is with methyloamine hcl your ethyl acetate lost 50% when u get freebase and then is much more faster made HCl ethyl acetate dmso NMP is the best way

 

[$!$]

Form 100g 2b4m
I get more like crystal powder like normal powder where normal get on dcm.
First is pure chemicals to get 84% no like much people 50% or 30%

 

[WillD]

Have you evaporated dcm?

 

[$!$]

Look Perfect 0 dirty shit 100% pure
40min work xD

 

[$!$]

Was no to much wet dry maximum 79% total crystal powder form 100g 2b4m
Later made ice glass crystal we see how much lost product on the scale