# Synthesis of 4-methylpropiophenone from toluene by Friedel-Crafts reaction (1kg+ scale)



## William Dampier (Sep 8, 2021)

*Reaction scheme:*





_Reagents:_
Propionyl chloride - 1000 g,
Toluene - 3000 ml,
AlCl3 anhydrous - 1500 g.

_Equipment:_
Flask,
Reflux condenser,
Drip funnel,
Distiller (straight condenser),
Mechanical stirrer.

All parts of the device must be carefully dried. Toluene applies anhydrous and taken in excess, as it serves as a solvent.

*Synthesis:*
1. In flask, equipped with a reflux condenser, a calcium chloride drying tube, drip funnel and mechanical stirrer, place aluminum chloride and toluene.
2. Start stirring and was added dropwise propionyl chloride with such speed, to the uniform release of hydrogen chloride.
3. In the case of a rapid reaction, outer cooling is needed.
4. The end of the reaction is determined by the cessation of hydrogen chloride.
5. After completion of the reaction, the reaction mixture was poured onto crushed ice and add a diluted hydrochloric acid solution to dissolve the aluminum hydroxide precipitate.
6. The top, benzene layer separated from the lower, water layer.
7. From the aqueous layer extracted with 4-methylpropiophenone with a small amount of benzene.
8. Benzene solutions are condensed and washed with a dilute solution of sodium hydroxide, water and dried magnesium or sodium sulfate.
9. After the toluene is distilled off to get 4-methylpropiophenone (mp 239 *С).


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## Oxygen

There was a alternative for mechanical stirrer?


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## Hans-Dietrich (Dec 4, 2021)

Oxygen said:


> There was a alternative for mechanical stirrer?



Oxygen
For example, what is the alternative ??? The volume of the reaction mass is approximately 5.5 liters, then the reactor is at least twice as large. Substances are extremely aggressive. I don't see any alternative. It is necessary to use a reactor (stainles steel) with a mechanical stirrer and a flue gas for synthesis. Protective suit (full body) with boots and gloves and a gas mask (complete head). It is also necessary to take into account the large amount of heat generated during the reaction.


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## Deedubbau

Hans-Dietrich said:


> For example, what is the alternative ??? The volume of the reaction mass is approximately 5.5 liters, then the reactor is at least twice as large. Substances are extremely aggressive. I don't see any alternative. It is necessary to use a reactor (stainles steel) with a mechanical stirrer and a flue gas for synthesis. Protective suit (full body) with boots and gloves and a gas mask (complete head). It is also necessary to take into account the large amount of heat generated during the reaction.



Hans-Dietrich
Mr. Safety to the rescue....

Yeah you better make sure you are wearing all that protective gear. Cause if you take this advise and use stainless steel you are going to have a disaster on your hands. Stainless is rapidly attacked by organic acids, and chlorides. So once you warm this mix up you better be prepared to run....or just stick with glass


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## Tony

Can you please make a video for synthesis , it will help me to synthesis mephedron , and it will help all beginners to make a mephedrone , it will be the most important video for me to make a mephedrone , because in my country i didn't find it to buy ( methylpropiopenone) so i have to synthesis it , and sorry for my English , i am from Egypt , my greetings  @William Dampier


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## Netflix

Buy 2b4m is legal in poland and is cheap


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## Tony

Netflix said:


> Buy 2b4m is legal in poland and is cheap



NetflixI am from Egypt , its unfortunately unlegal to buy it , It is forbidden to sell in Egypt...Can you help me somehow?


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## hlebsladky2

William Dampier said:


> *Reaction scheme:*
> View attachment 1289
> 
> _Reagents:_
> ...



William DampierWhat's the possible yield?


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## G.Patton

hlebsladky2 said:


> What's the possible yield?



hlebsladky290-95%


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## estimated

hello, can toluene be replaced with xylene?


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## G.Patton

Probably yes



estimated said:


> hello, can toluene be replaced with xylene?



estimated


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