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4-MMC Complete Synthesis

Brinda

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4-MMC Synthesis

Big thanks to @WilliamDampier for providing me with the necessary reagents to synthesize this compound.

Abstract
4-MMC is a synthetic stimulant of the amphetamine and cathinone classes. It is chemically similar to the cathinone compounds found in the khat plant of east africa.
It produces effects similar to MDMA, Amphetamines and Cocaine. In addition to its stimulant effects it also has side effect, one of which is bruxism (most common). Effects of 4-MMC has been studied in rats and humans and the metabolites can be detected in urine after uasage.

Background
4-MMC was first synthesiszed in 1929, but was not widly known untill the early 2000’s at which point it was rediscovered. At the time its was legal to buy and sell in most countries however its is now illegal to synthesize, posses, distribute and use. As of July 2012 the United States permanently classified this as a Schedule 1 drug under the Synthetic Drug Abuse Prevention Act (SDAPA).

Formula: C11H15NO
Molar Mass: 177.247 g/m
IUPAC Name: (RS)-2-Methylamino-1-(4-methylphenyl)propan-1-one


Reaction: 1C10H11BrO+1CH3NH2=1C11H15NO+1H+1Br
Reaction Mechanism: Double Replacement

Synthesis
In a 1000ml RBF 1 Mole of 2-Bromo-4-Methylpropiophenone was dissolved in 1 Mole of Dimethylbenzene. The solution was then placed and a magnetic stirrer and hotplate and allowed to stir until all reactants were completely dissolved.

Following the dissolution of the 2-Bromo-4-Methylpropiophenone in (CH3)2C6H4, 1 Mole of Methylamine (CH3NH2) was weighed and dissolved in 50ml of H2O. This solution was then added to a 100ml pressure equalizing addition funnel. The addition funnel was then attached to the 1000ml RBF and addition commenced at a rate of 1 drip per second. The magnetic stirrer was turned on to allow even distribution of CH3NH2 in solution.

Once all CH3NH2 was added, heating was turned on and temperature was kept at a constant 35 degrees celsius. The solution was left to react for 5 hours or until a deep red/amber color was observed.

Heating was then turned off and solution was left to separate and cool. Once solution has cooled to room temperature the aqueous layer was separated from the solvent layer making sure to keep the solvent layer in a adequate storage bottle until further use. The remaining aqueous layer was extracted with 100ml of (CH3)2C6H4 and an emulsion was formed. Layers were then allowed to separate and solvent layer was kept and aqueous layer was discarded.

Both solvent layers were combined and added to a 500ml beaker. 150ml (excess) of HCL was then slowly added to the solution to form 4-MMC HCL.

Solution was then vacuum filtered to extract any precipitated 4-MMC and purify the product. Filtrate was then collected and evaporated by rotary evaporation until the crude product was obtained.

Recrystalization was done by dissolving the product in a 50/50 solution of EtOH and H2O and then allowed to evaporate to form a more pure product. Further purification can be done by column chromatography with SiO2 leaving the purity at around 99.89-99.988%.







2024 RaidChem/Brinda
 

JustBrowsing223

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@Brinda Thanks for sharing!

Did you use reflux condenser while keeping temperature at 35? Im just wondering if its necessary as xylene bp is 138c (atleast according to wiki).
What was the yield?
Also, what as the concentration of HCL?
 

Brinda

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@Brinda Thanks for sharing!

Did you use reflux condenser while keeping temperature at 35? Im just wondering if its necessary as xylene bp is 138c (atleast according to wiki).
What was the yield?
Also, what as the concentration of HCL?
JustBrowsing223HCL was at 32%
I've also tried to use a reflux condenser but xylene is so volatile that it does not really help. I just either use a reflux condenser with aluminum over the top or I just use aluminum.
There does not seem to be much of a difference.
 
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