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?

 

[PharmacopeiaLabs]

HCL in Ethyl Acetate will also begin an Acid Catalyzed Hydrolysis of the EA, this is why as far as i understand its mandatory to distill all EA and replace it with Acetone before Acidification.

 

[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?

 

[WillD]

Unless you use some correction and modifications to the method. Such as anhydrous methylamine and additional distillation. Also, you can use NMP synthesis for scaling, but that's more expensive.

 

[PharmacopeiaLabs]

why do we discard the methylamine water 20 minutes after its addition?

 

[Dr. MMX]

bevcasue there is nothing to do you don t want tin product right

 

[PharmacopeiaLabs]

i wasn't aware that the reaction is complete in 20-30 mins when using EA, i will not delete it tho in case someone else has the same question in the future