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Lets start discusing.

I know few synth methods of 4MMC from bromketone (i am not interested in


bromketone synth methods lets not discus abut them):

1) Kinetic method, mistake in this method is that there is lot of methylamine salt in product and when
you adding HCl (aq), there is formating blue shit (washed away with acetone and get white product, but
what it is?). Also interesting is that blue collor can get away with powerfull oxiders. Higest yield was
using methylamine gas and HCl gass.

To a stirred solution of 11.4g (50mmol) 2-bromo-4’-methylpropiophenone in 25mL toluene held at 20oC


was added, over 5 minutes, 6.2g methylamine in 35mL water (prepared by adding a solution of 7.9g
(198mmol) sodium hydroxide in 20mL cold water to a cooled solution of 13.5g methylamine HCl in 15mL
water). The mixture was allowed to stir for a further 16 hours at 20-25oC, then was poured into 150mL
ice-cold water. The toluene layer was separated off, and the remaining freebase extracted with 2x20mL
toluene. The combined toluene extracts were washed with 3x25mL water, and then acidified with
2x15mL dilute HCl. The combined acidic extracts then washed twice with 25mL toluene and evaporated
under vacuum to dryness, allowing an off-white solid to form. 20mL acetone was added and was heated
to boiling, forming a homogenous solution, which was then slowly cooled, allowing crystals to
precipitate. The crystals were filtered and rinsed with around 100mL ice cold acetone.

Yield: 4.8g (45%)[/i][/i]

2. Russian method

20g substrate was disolved in 100mL benzene

added 20g NaOH in 100mL H2O

added 40mL mehylamine (aq solv).

2h boiled with reflux

Added HCl in dioxane, filtered.

Mildronate comments: when using hcl aq solv red shit forming washed awa with acetone. What is
orginal paper (literature) for this method?
Anothe method from internet also writed in wiki, what is original papaer for this (literature)?:

4-Methylmethcathinone

1.0 g of the 40-methyl-2-bromopropiophenone (4.4 mmol)was dissolved in 30 mL of CH2Cl2 and added


dropwise over an hour to a stirred solution of 0.3 g ofmethylamine hydrochloride (4.4 mmol) and 1.0 g of
triethylamine (9 mmol) in 50 mL of CH2Cl2. After the addition was complete the mixture was stirred at
room temperature for 4 h. 100 mL of aqueous HCl was added and the aqueous layerwas removed
andwashedwith 40 mL of CH2Cl2. The aqueous layer wasmade alkaline with a solution of NaOH and the
amine was extracted into 2 x 50 mL of CH2Cl2. The CH2Cl2 was evaporated under vacuum and the
resultant oil was dissolved in anhydrous ether. HCl gas was bubbled through the ether to produce the 4-
methylmethcathinone hydrochloride. The hydrochloride salt was recrystallised from iPrOH. The yield of
4- methylmethcathinone hydrochloride was approximately 30%

3) 4MMC synth was first reported i French yournal (Saem de Burnaga Sanchez, J. (1929). "Sur un
homologue de l'éphédrine [On an analogue of ephedrine]" (in French). Bulletin de la Societé Chimique
de France 45: 284–286), and there was only one synth method for 4MMC in reaxys, this Sanchez
method:

Methylamine is reacted in benzene solution.

240 ml. of a solution of 8% monomethylamine in bromoacetone from 40 g of p-toluylethylacetone.

The reaction is very strong, even at room temperature. It quickly separates monomethylamine
hydrobromide crystals. We abandone the mixture itself overnight, the crystals are separated on
hydrobromide monomethylamine and hunting most of the solvent. The residue is taken up in water and
dilute hydrochloric acid until neutralization in tornesol. The aqueous layer is decanted. Washed with a
few benzene. The solution is decolorized by animal charcoal and saturated with sodium carbonate;
based release is extracted with ether. The ether solution is then treated with water and hydrochloric
acid, to separate the base to the hydrochloride, then the aqueous solution is evaporated in a vacuum.
The residue is crystallized, washed with acetone and anhydrous ether and recrystallized in absolute
alcohol and acetone, 232 º F, R 45%.[/i]

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