Method for preparing gamma-tertiary butyl-chlorobenzene butanone
The technology of chlorophenbutanone and tert-butyl group is applied in the field of preparation of important pharmaceutical intermediates, and can solve the problems of waste of raw material consumption, high production cost, increase of product preparation cost and the like
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[0012] 1. Acyl chloride reaction stage: In the cleaned and dried reaction kettle, suck in butyrolactone, put in zinc chloride under stirring (zinc chloride needs to remove water), after feeding is completed, heat up to 35°C and keep it for 1 hour, then cool down At 20°C, start to add thionyl chloride dropwise, and control the temperature to 30-35°C. After the dropwise addition, raise the temperature to 40°C, keep it warm for 1.5 hours, raise the temperature to 50°C and keep it for 1 hour, raise the temperature to 55°C and keep it for 1.5 hours, raise the temperature to 65°C, keep it for 2 hours. To obtain semi-finished butyryl chloride.
[0013] Wherein the feeding ratio is: butyrolactone=100kg
[0014] Zinc chloride = 15kg
[0015] Thionyl chloride = 250kg
[0016] 2. Hydrolysis stage: put dichloroethane and aluminum trichloride into the cleaned reactor and stir to lower the temperature to -5°C, start to add butyryl chloride dropwise, contro...
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