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This video represent a simple synthesis way of 4-MMC (mephedrone) in a small scale from 4'-methylpropiophenone. There is total synthesis video manual which explain everything and gives opportunity to make 4-MMC to every beginner of organic synthesis.

Equipment and glassware:
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Reagents:
  • 4'-Methylpropiophenone (cas 5337-93-9) - 100g;
  • Benzene – 600ml;
  • Bromine (Br2) - 100g;
  • N-methylpyrrolidone - 300ml;
  • Methylamine free base 40% (aqueous solution) - 200 ml;
  • Hydrochloric Acid 35% - 55ml;
  • Acetone - 1000ml;

Description of the 4-MMC (mephedrone) synthesis video:
From 0:00 to 0:48
It is said at the start of this video that laboratory and reagents temperature (except for those that need to be cooled) should be moderate, about 20-25ºC.

Next, the preparation of the reactor to work is described:
"2000ml Round bottom flask is placed on a magnetic stirrer and secured to a retort stand and clamp for securing apparatus. A magnetic stirrer work is checked. Reflux condenser is installed on the central flask neck and a gas outlet hose is fit to it. The hose is installed carefully, without kinks. The end of the hose is immersed into a canister with 15% aqueous sodium bicarbonate solution (to absorb odors)."

Then, the reagents loading is come :
""4-Methylpropiophenone 100g and benzene 300ml are poured into the flask and stired. Bromine 100g and benzene 100ml are poured into the drip funnel. A thermometer is installed and bromine is dropped into a reaction mixture. A gentle heating is turned on and the temperature in the flask is increased to 35 ºC, then the heater is turned off."


From 0:48 to 3:23
Bromination reaction. The bromination is started by a chemist after the all reagents loading. Bromine solution is added in small portions to benzene in the flask, so that the reaction mixture has time to discolour. After the bromine addition, the mixture is stirred on a magnetic stirrer for addition 30 minutes.
"Bromine is added drop by drop to the mixture in four equal portions after the switching off the heater . Each further bromine portion is added after discoloring of previous one."
"The reaction mixture is stirred for additional 30 minutes after complete bromine addition"
The 4-Methylpropiophenone bromination gives 2-bromo-4-Methylpropiophenone in benzene.


From 3:23 to 6:16
Reaction mixture is
washed in separatory funnel and excess pressure is revealed through a tap. The funnel is twisted in a circular motion, for collecting the remaining water and draining it, the solution of 2-Bromo-4-Methylpropiophenone in benzene is left for the following synthesis.
" Water 200 ml is added after 30 minutes."
"The mixture is poured into the separatory funnel. Layers are separated clearly. The bottom layer is disposed, the top layer is needed."
"The washing is repeated. Water 200 ml is poured and shaken well. Layers are separated clearly. The bottom layer is drained.
Do not forget to release the pressure by opening the tap."
"The funnel is rotated in a circular motion to collect all water in the bottom layer."


From 6:17 to 9:02
Methylamination reaction. The solution of 2-Bromo-4-Methylpropiophenone in benzene is poured back into the flask, methylamine is poured. The reaction mixture is heated to 40 ºC. NMP is added in small portions, make sure theat a temperature is not exceeded 60 ºC. In case the temperature is exceeded 60ºC, the following addition have to be carried out when temperature is droped. After all NMP has been added, the reaction mixture is stirred for 15 minutes. A rich amber color of the reaction mixture can be observed during the methylamination process. This is a sign that the reaction is over.

2-Bromo-4-methylpropiophenone methylamination gives mephedrone free base (4-MMC).
"The obtained 2-Bromo-4Methylpropiophenone in benzene is poured back into a clean flask and 40% methylamine 200ml (aqueous solution) is added."
"A reflux condenser, drip funnel and thermometer are installed onto the flask. The stirrer is turned on and flask is heated to 40 ºC."
"When the temperature is reached 40ºC, the heater is turned off and N-methylpyrrolidone 300 ml is added from the drip funnel, make sure that the temperature is not exceed 60 ºC. A short exothermic reaction takes place and the temperature can rise after addition of N-methylpyrrolidone."
"Reaction mixture is stirred for 15 minutes after all N-methylpyrrolidone is added."


From 9:03 to 11:33
Mephedrone free base washing. The free base is washed with sodium bicarbonate solution 200ml 5% and water 3 x 200ml . The mixture is shaken well, an excess gas pressure is released through a tap. Layers are separated clearly in the separatory funnel. The lower aqueous layer is drained into a waste, the upper organic layer with a free base is left for further work. A pinch of sodium chloride is added to solution for residual water removing from a turbidity. It is left for some time after well stirring to layer separating and a water residue is drained. The pure free mephedrone base is obtained.
"Then sodium bicarbonate solution 100ml 5% and benzene 200ml are added, stirred well, poured into a separatory funnel. Layers are separated clearly."
"The lower water layer is disposed off"
"Water 200 ml is poured to mephedrone free base in benzene (top layer), stirred well. Layers are separated clearly. The lower aqueous layer is disposed off."
"Mephedrone free base in benzene is washed with water three times."
"If mephedrone free base solution in the benzene looks cloudy after washing, some sodium chloride is added and stirred in a circular motions."
"The mixture is left to stand for a couple of minutes, the rest of the water with the sodium chloride is collected at the bottom layer. This water residue is disposed off. Pure mephedrone free base in benzene is remained in the funnel."


From 11:34 to 12:38
Acidification. Mephedrone free base is converted to hydrochloride salt in this part of the synthesis. Hydrochloric acid is added drop by drop to 4MMC free base with a constant stirring. The solution is become hot after acidification and precipitate is appeared. This precipitate is mephedrone hydrochloride. It is necessary to measure pH constantly during the acidification procedure. The acidification is stopped when pH 5-5.5 is reached. The beaker with mixture is covered with a film and put into a freezer for a few hours.
"Mephedrone base in benzene is poured into a wide beaker, put it on a magnetic stirrer. A stirring bar is placed inside and stirring is started. A drip funnel is placed above the beaker and hydrochloric acid 55 ml is added at 1-2 drops per second rate."

"pH is measured every 10 seconds to reach 5-5.5 pH. Mephedrone hydrochloride is formed in the beaker and the temperature is rise during the acidification procedure. Mephedrone hydrochloride can be dissolved, this situation is normal. Crystalls are appeared during a cooling procedure."

"The stirrer is turned off when pH is 5-5.5, the beaker is covered with a cling film and put it in a freezer for 4 hours. The freezer temperature shouldn't be lower than -15 ºC."


From 12:39
Filtration and washing.
The
filtration apparatus is prepared: Buechner funnel with a paper filter is placed on a Buechner flask in the final part of the video. The filter is moistened with acetone for a better contact with a funnel surface. The mixture is stirred well so that the precipitate does not stick to a beaker and poured into the funnel. The mephedrone remainder is washed off with an additional portions of acetone and transferred to a Buechner funnel.

Then a vacuum pump is connected to Buechner flask via a hose. The powder is thickened slightly and cracks are appeared during the filtration process. A small amount of acetone is added to the Buechner funnel, switching off the vacuum at the same time, for the better washing and purity level. The product is washed with acetone until transparent flushes is started to drip from the funnel.

The powder is dried in Buechner funnel with a switched on vacuum until mephedrone hydrochloride powder is become crumbly after washing with acetone. The mephedrone is air dried in a dry room and weighed.
"The resulting precipitate is filtered under vacuum and washed on the filter with acetone.
The long edge of the funnel spout in the opposite direction from the side outlet of the flask is unfolded."
"The filter have to be moistened with acetone."
"The mephedrone powder residue in the beaker is washed off with portion of acetone."
"Hose from a vacuum pump."
"Magnet from a magnetic stirrer."
"Mephedrone is dried on the air. The theoretical yield of mephedrone hydrochloride is 144g from 100g of 4-methylpropiophenone, but considering losses, you get ~100g (maybe more)."
 
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lolman172

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thanks mate video was amazing. but i need to ask you that its really hard to find 4-methylpropiophenone this sht here. what can i do ? instead of this chic ?
 

2FDCK-chef

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thanks mate video was amazing. but i need to ask you that its really hard to find 4-methylpropiophenone this sht here. what can i do ? instead of this chic ?
lolman1724-methylpropiophenone 1451-82-7
Is it this product?
 

Jamroz

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I got ready 2-bromo-4-methylpropiophenone. In what amount of benzen i need to disolve it for this reaction? Can i exchange nmp for another solvent? If yes can you give me some examples of scale
 
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The reaction with NMP takes 15-20 minutes, it can be replaced by Dimethyl sulfoxide, Dimethylformamide or Sulfolane.
But NMP is the best choice.
For 1g of 2-bromo-4-methylpropiophenone you take 3ml of benzene, if not completely dissolved you can add 1-2ml. The reaction takes much longer in benzene. If you don't heat the mixture, reacts for ~24 hours, depending on the amount of ketone.
 
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ELOELO

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The reaction with NMP takes 15-20 minutes, it can be replaced by Dimethyl sulfoxide, Dimethylformamide or Sulfolane.
But NMP is the best choice.
For 1g of 2-bromo-4-methylpropiophenone you take 3ml of benzene, if not completely dissolved you can add 1-2ml. The reaction takes much longer in benzene. If you don't heat the mixture, reacts for ~24 hours, depending on the amount of ketone.
Marvin "Popcorn" SuttonThis will be my first time due to my lack of experience in chemistry, I would like to make sure of something. Starting with 2b4m, is it enough that I dissolve them in 300ml of benzene and, after complete dissolution, add 200ml of methylamine? Methylpyrrolidone is not required in my case?
 

dark_side_of_chemistry

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hello, i have a question about the amination stage. Is bk4 better to dissolve in nmp and add methylamine as described in Synthesis of mephedrone in NMP (large scale) or to dissolve in toluene, for example, add methylamine and then only nmp as in the video?
 

Jamroz

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I try react 100g 2-bromo4methylpropiophenone with proportion 200ml methyloamine 40% and 300ml nmp.Finish yield was 40g mephedrone hcl but i add to much acid ph paper was light red ph under 5 but just a little bit.How much g schould i get from 100g 2bromo4propiophenone ? How much acid schould i use per 100g bromoketone ?i want to try 25kg scale ,schould it work in your opinion ?
 
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I understand correctly that you want to react 25 kg of 2bromo4propiophenone? That's quite a big volume, but it's realistic. Approximate consumption of hydrochloric acid is 300-400ml per 1 kg of 2bromo4propiophenone.
 
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Jamroz

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Can you tell me how much g of mephedrone should i get from 100g 2bromo4propiophenone if i do it correctly?
 
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C10H11BrO + CH5N → C11H15NO + HBr
As can be seen from the equation, one molecule of 2-bromo-4-methylpropiophenone produces one molecule of mephedrone.
C10H11BrO : 227.0977 g/mol
C11H15NO : 177.2429 g/mol
227.0977/177.2429=1.28127953
The coefficient is 1.28127953
This means that from 100g of 2-bromo-4-propiophenone, you will get 78.0469818g of mephedrone base.

The mass of mephedrone hydrochloride will increase by 1.19 g/cm3 and the coefficient will be 1.27273446
C11H15NO+HCl=177.2429+1.19=178.4329
227.0977/178.4329=1.27273446

100g(C10H11BrO)/1.27273446=78.5709849g(C11H15NO)
The theoretical yield of the reaction of 2-bromo-4-methylpropiophenone was 78.5709849g mephedrone hydrochloride. But it should be considered that it is difficult to achieve the theoretical yield, usually the loss is 20%.
 
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delkibrother

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In the video the final result is a powder, is it possible to achieve a solid "rock"?
Per my understanding we can say that generally the final yield is around 70-80% of the 2-bromo-4-propiophenone used?

And also: if I already have 2-bromo-4-methylpropiophenone, then what will change in the video process?
 
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In the video the final result is a powder, is it possible to achieve a solid "rock"?
delkibrotherThis is the next step after receiving the powder.
Per my understanding we can say that generally the final yield is around 70-80% of the 2-bromo-4-propiophenone used?
Up to 78% is the theoretical yield, the actual yield is ~60% of the mass of 2-bromo-4-methylpropiophenone .
And also: if I already have 2-bromo-4-methylpropiophenone, then what will change in the video process?
2-Bromo-4-methylpropiophenone should be dissolved in benzene, methylamine should be added and NMP should be added little by little.
 

Jamroz

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Canlyou tell me what can i use instead of benzen? Its difficult to get it in large scale.
 

btcboss2022

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Hello,

I should replace NMP by DMF in the same amount?

Thanks.
The reaction with NMP takes 15-20 minutes, it can be replaced by Dimethyl sulfoxide, Dimethylformamide or Sulfolane.
But NMP is the best choice.
For 1g of 2-bromo-4-methylpropiophenone you take 3ml of benzene, if not completely dissolved you can add 1-2ml. The reaction takes much longer in benzene. If you don't heat the mixture, reacts for ~24 hours, depending on the amount of ketone
Marvin Popcorn Sutton
 

karamelosanto

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Hi!
Can I replace NMP with DMSO (Dimethyl sulfoxide)?
If so, what amound I would need?

Also apart of benzene, toluene, xylene, DCM, ethyl acetato, what else can I use?
Thanks
 

btcboss2022

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Hello I did it with DMF and Toluene.
 
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Hi!
Can I replace NMP with DMSO (Dimethyl sulfoxide)?
If so, what amound I would need?
karamelosantoStick to the same proportion as the NMP.
DMSO, DMF, NMP and Sulfolane are interchangeable solvents. They are used as a solvent, creating a medium for a fast reaction. The proportions can be changed, but then the volumes of the other solvents used must be adjusted as well.
Also apart of benzene, toluene, xylene, DCM, ethyl acetato, what else can I use?
Thanks
It is better to use these solvents, they are tested and work very well. But it is possible to use other solvents, you need to check their properties as they will work with the available reagents.
 
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