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

Inactive Publication Date: 2010-05-05
扬州市天平化工厂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The production cost of the previous r-tert-butyl-chlorobutyrophenone was high, which greatly affected the further promotion of its use and dosage
In the prior art, the residue after the acylation reaction is often treated as solid waste directly, which reduces the yield of the product, wastes the consumption of raw materials, and increases the treatment cost of "three wastes" and the discharge of "three wastes" with the total amount, which increases the preparation cost of the product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment Construction

[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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PUM

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Abstract

The invention relates to a method for preparing gamma-tertiary butyl-chlorobenzene butanone. The method is characterized by comprising the following steps of: (1) acylation reaction: sucking butyrolactone into a clean and dry reaction kettle and strring, and then adding zinc chloride into the reaction kettle for reaction to generate semi-finished butyl chloride; (b) hydrolysis reaction: adding dichloroethane and aluminium choride into a clean and dry reaction kettle, dropwise adding the butyl chloride into the reaction kettle while stirring; then continuing to dropwise adding tedin benzene , and steaming off dichloroethane to generate the gamma-tertiary butyl-chlorobenzene butanone. 3gamma-tertiary butyl-chlorobenzene butanone products prepared by the method are pale yellow granules, wherein the content of the 3gamma-tertiary butyl-chlorobenzene butanone is more than or equal to 90 percent, and the pH value is larger than or equal to 3.85. The reaction process of the method is easy to control, the utilization rate of raw materials and the yield of the products are improved, and the method conforms to the requirements on environmental protection and cleaner production and improves the economic benefits of enterprises.

Description

technical field [0001] The present invention relates to a kind of preparation method of important medicine intermediate, especially a kind of preparation method of r-tert-butyl-chlorobutyrophenone. Background technique [0002] r-tert-butyl-chlorobutyrophenone is a pharmaceutical intermediate mainly used in the synthesis of teferidine antiallergic drugs, and the antiallergic drugs made from r-tert-butyl-chlorobutyrophenone can be Effective anti-allergic, anti-allergic mechanism is special, the dosage is small, and the drug effect is remarkable. The production cost of the previous r-tert-butyl-chlorobutyrophenone was high, which greatly affected the further popularization of its use and dosage. In the prior art, the residue after the acylation reaction is often treated as solid waste directly, which reduces the yield of the product, wastes the consumption of raw materials, and increases the treatment cost of "three wastes" and the discharge of "three wastes" With the total ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/80C07C45/68
Inventor 马文元许广岭张兴华
Owner 扬州市天平化工厂有限公司
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