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]

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?

DavidNicholsHaving 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]

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?

Chemix-ExpressYes, 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]

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.

Chemix-Express40 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]

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).

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

 

[w2x3f5]

del

 

[DavidNichols]

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

w2x3f5

and why 4-mec (n-ethylcatinon)???

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]

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

w2x3f5Addition to 4-MEC formation under extended reaction time under reflux in alkaline environment:

It is known that both cathinone and
methcathinone are rather unstable as free bases in alkaline conditions giving rise to a series of decomposition products (benzaldehyde, ethylamine, phenylpropanedione and a pyrazine dimer).

 

[w2x3f5]

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.

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

 

[w2x3f5]

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

DavidNicholsIn 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]

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.

Chemix-ExpressYou 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]

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

UWe9o12jkied91dIn 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]

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

UWe9o12jkied91dI don't think that it is good idea.

 

[DavidNichols]

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

UWe9o12jkied91d

Any idea if sodium hypochloride

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

 

[w2x3f5]

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

DavidNicholsHypochlorite 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.