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

William Dampier

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Reaction scheme:
H0AOG9Lmgc.png


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

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There was a alternative for mechanical stirrer?
 

Hans-Dietrich

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There was a alternative for mechanical stirrer?

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.

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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