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

[yin-yang]

I didn't try this reaction yet. I watched video published here iodo-ketone amination. There I saw freebase is black and powder changed colour when preparing for crystalization. Maybe it was black cause of iodine being leaving group as opposed to bromine.
Questions to comfirm:

1. Results above are from ethyl acetate as a solvent ?
2. Have you done this reaction with EA and bromoketone, does freebase look any different?
3. I noticed from video that crystals from EA look glass like, while NMP are lot whiter. I read your post about stereochemistry of 4-MMC how S and R enantiomers form different looking crystals, are both of these crystals equally racemic?
4. Did you notice any difference in subjective effect between EA and say NMP in final product?

Thank you for posting these results.

 

[DavidNichols]

Can you please link me that post?

 

[Rush-Benzo]

Using ready-made BK4 how much should I give it for a 2L m40?

 

[G.Patton]

Hello, you can increase amount of reagents proportionally. Read Moles, grams, litres and chemical calculations topic.

 

[G.Patton]

What yield did you get? Same?

 

[karate.kid]

What is theorethical yield before recrystallization?

 

[mocnykutas]

55%

 

[RegulierTier]

Would this work for Methamphetamine as well?

 

[RegulierTier]

What's so funny with that? I mean, the only difference is that the 4-mmc precursor is a ketone and n-propylbenzene is not. So why might this not work with the missing O-doublebinding?

 

[RegulierTier]

i'm just curious

 

[RegulierTier]

The structure of both substances does not differ greatly. The only difference between Mmc and Meth is that one is a ketone and the other is not. Additionally, the oxygen double bond does not participate in the reaction. So why shouldn't the synthesis route work for Meth as well? Just because it's not the same substance doesn't mean that the synthesis route wouldn't work for both substances. The synthesis should also be transferable to other precursors.

 

[G.Patton]

Hi, actually they are different and ketone group is very important. Oxygen with sp2 hybridization withdrawn electrons from C2 atom and allow to carry out such nucleophilic addition reaction with HBr.

 

[RegulierTier]

Ah ok that makes sense, thanks.

 

[mocnykutas]

Real easy synthesis.

 

[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?

 

[mocnykutas]

Acetone and ethyl acetate is good.but toulen is shit to made mmc

 

[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.

 

[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]

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.

 

[mocnykutas]

On toulen 60° and 2h the same and much more need heat

 

[Chemix-Express]

3h at 60 degrees gives the best result. But not about that. At 60 degrees Toluene does not boil, while DCM at 40 does, hence it evaporates quickly and a reflux cooler is needed. Isn't it?

 

[mocnykutas]

I dont use lab equipment i dont know.

 

[mocnykutas]

Im made in 20min freebase

 

[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]

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.

 

[Chemix-Express]

I know how it should look.

4CMC