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

WillD

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Reaction scheme:
H0AOG9Lmgc


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).
 
Last edited by a moderator:

Oxygen

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There was a alternative for mechanical stirrer?
 

Hans-Dietrich

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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

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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
 

The-Hive

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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
DeedubbauI use stainless steel vessel for larger reactions so far so good IMO
 

Tony

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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
 

Netflix

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Buy 2b4m is legal in poland and is cheap
 

Tony

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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?
 

hlebsladky2

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Reaction scheme:
View attachment 1289

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).
William DampierWhat's the possible yield?
 

estimated

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hello, can toluene be replaced with xylene?
 

plancklong

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hello, can toluene be replaced with xylene?
estimatedNo. The toluene is not just the solvent. It is the basis for the 4-methylpropiophenone:

XFJZp7u8Yi


Which xylene did you have in mind, o, m, or p? Never mind, it's probably a mixture of all 3:

VjTNtYQsw1


If you did use these, can you see that you would NOT be synthesizing 4-methylpropiophenone?
 

reza

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After the completion of the reaction, the reaction mixture was poured onto crushed ice and diluted hydrochloric acid solution was added to dissolve the precipitate of aluminum hydroxide. Step five is a bit
Could you please explain more, do you mean to put the container of the reaction mixture in a container of ice? How much concentrated hydrochloric acid?
 

UWe9o12jkied91d

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After the completion of the reaction, the reaction mixture was poured onto crushed ice and diluted hydrochloric acid solution was added to dissolve the precipitate of aluminum hydroxide. Step five is a bit
Could you please explain more, do you mean to put the container of the reaction mixture in a container of ice? How much concentrated hydrochloric acid?
reza
After the completion of the reaction, the reaction mixture was poured onto crushed ice and diluted hydrochloric acid solution was added to dissolve the precipitate of aluminum hydroxide.
The reaction mixture itself, not the container.The ice water will help dissolve soluble impurities aswell as cool down the exotherm from HCl reacting with aluminium compounds.
Dosent matter much as to my interpretation, it is done to dissolve the aluminium residues, which can create a gunk at the interface that is hard to separate fully.Add until residues are dissolved and I think you can use any conc. HCl, taking care if adding conc., that’s all.
 

Frit Buchner

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Man! If anyone know a source or easy synth for propoinyl chloride?
 

Frit Buchner

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📨
 

reza

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Is distillation in a vacuum meant? I don't have a rotary evaporator, do I need one?
 

UWe9o12jkied91d

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Is distillation in a vacuum meant? I don't have a rotary evaporator, do I need one?
reza4-methyl propiophenone is somewhat stable in air as far as I know, so you could let the toluene just evaporate if you wanted to
 

reza

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Does it mean I don't heat? Don't you think it will take a long time to completely evaporate?
Thank you for your opinion and advice
 

UWe9o12jkied91d

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Does it mean I don't heat? Don't you think it will take a long time to completely evaporate?
Thank you for your opinion and advice
rezaYes, it's possible, toluene evaporates quite fast even at RT.
You can also heat gently on a water bath
 
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