Síntese de 4'-metilpropiofenona a partir de tolueno por reação de Friedel-Crafts (1kg+ escala)

Deedubbau

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Sr. Segurança para o resgate....

Sim, é melhor certificar-se de que está a usar todo o equipamento de proteção. Porque se seguir este conselho e utilizar aço inoxidável, vai ter um desastre nas suas mãos. O aço inoxidável é rapidamente atacado por ácidos orgânicos e cloretos. Por isso, quando aqueceres esta mistura, é melhor estares preparado para correr.... ou então fica com o vidro
 

amieri

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"let me show you something"
 

NovicechemistEU

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Tomorrow I'm starting the big day synthesis with a small batch.
I wanted to start with a small batch for my first try.
1.08 mol 100 Gr 95.2 mL propionyl chloride
1.12 mol 150 Gr: AlCl₃
2.81 mol 300 ml 261 Gr Toluene
I can use 50 ml more toluene. 350 ml
Toluene of 99.5% purity was dried and then distilled under vacuum. We follow the advice of the masters :)
 
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Smokesalot99

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Can you replace propionyl chloride with propionic anhydride for reaction?
 

The-Hive

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try it and let us no do it on a small scale then compare it to using propionyl chloride
 

William D.

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Do you think this reagent is more easy to buy? And cheaper? I think this is not so, but if you have it, you can go with such a route but with correction.
 

NovicechemistEU

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I finally managed to make the synthesis, I can't thank @William D. enough for helping me every step of the way, I am very grateful :)
Now I just need to distill the dirty 4'-methylpropiophenone under vacuum :)

2K0tGAYRp9
 

Jack

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Here's a paper on the synthesis of 4 methyl propiophenone with AlCl3 and propionic anhydride with includes a procedure https://www.pismin.com/10.1248/cpb1953.4.182 . Studies on the Syntheses of Ring Substituted p-Alkylephedrines and p-Alkylnorephedrines. Pharmaceutical Bulletin, 4(3), 182–188. (1956)
 

Jack

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Propionic anhydride is a better acylating agent since for an amateur to obtain a acid chloride without phosphorus chlorinating agents would involve going through carboxylic acid anhydrides anyway.
 
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