# Oxidative alpha-Amination of 4-methylpropiopnenone with Ammonium iodide



## William Dampier (Jul 23, 2021)

*Reaction scheme:*





*Synthesis:*
1. NH4I (15 g) was added to a mixture of sodium percarbonate (200 g), 4-methylpropiophenone (100 g), and methylamine (200 ml 40%) in DMF (600 ml) at room temperature.
2. The reaction was stirred at 50 *C 18 hours.
3. The reaction mixture was then allowed to cool to room temperature, dilute water (1500 ml).
4. Extracted with benzene (500 ml).
5. Acidified 5:1 solution conc. HCl in IPA to pH=5.
6. Crystallisation in cold 12 hours and filtered in vacuum, washing cold acetone and dry.


----------



## ADATA

This way directly 4MMC without bromination?
Are there any other alternatives to DMF?
acetone?


----------



## G.Patton

ADATA said:


> acetone?



ADATAmethylamine will react with acetone


----------



## ADATA

Are there any other options besides DMF?


----------



## William Dampier

ADATA said:


> Are there any other options besides DMF?



ADATADMSO and acetonitrile maybe.


----------



## ADATA

I will try the 4MMC harvested from this program
How much output can 1KG produce?


----------



## William Dampier

For some reasons, the reaction poorly scale, start with a small scale


----------



## ADATA

Is 1000G scale possible?


----------



## William Dampier

ADATA said:


> Is 1000G scale possible?



ADATAMaybe, but start with smaller quantities. In general, the synthesis of the intermediate and its subsequent use is the best option than this synthesis.


----------



## karamelosanto

Hi, I have a few questions about this route.
Methylamine 40% solution is in water or methanol ?
Can benzene be replaced with hexane or DCM or another solvent?
For scale this down like on the range of 10g 4-mpf. Is correct to scale down all the others reagents in the same 10/1 way?
Thanks


----------



## G.Patton

karamelosanto said:


> Methylamine 40% solution is in water or methanol ?



karamelosantowater


karamelosanto said:


> Can benzene be replaced with hexane or DCM or another solvent?


yes, you can all of them. Also can use Petroleum ether


karamelosanto said:


> For scale this down like on the range of 10g 4-mpf. Is correct to scale down all the others reagents in the same 10/1 way?


dev 10


----------



## zyuxo0

Is this a good procedure to start my adventure with organic chemistry? Or should I start with classic halogenation?

I will do only nano scale. And I want to try because it looks like I can make a lot of experimental cathinones and this turns me on haha

What are the disadvantages of this procedure?

I know these are dumb questions for pros but anyways...


----------



## Mellym

I guess this should work with carbamide peroxide (hydroperite) instead of sodium percarbonate.
Overall this scheme looks quite messy to me..


----------

