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1-hydroxy cyclohexyl phenyl methanone synthesis process

A technology of hydroxycyclohexyl phenyl ketone and synthesis process, which is applied in the field of synthesis technology of 1-hydroxycyclohexyl phenyl ketone, can solve the problems of low production efficiency, unsuitability for large-scale production, complicated production process and the like, and achieves Improve work efficiency, improve single-pass conversion rate and product yield, and overcome the effect of many processes

Inactive Publication Date: 2016-06-08
吕艳
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  • Summary
  • Abstract
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  • Application Information

AI Technical Summary

Problems solved by technology

In the current synthetic process method of 1-hydroxycyclohexyl phenyl ketone, the technical process is not easy to implement, the resulting 1-hydroxy cyclohexyl phenyl ketone has low purity, the reaction residue cannot be recycled, and the production process is complicated. Low production efficiency and high cost, not suitable for mass production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0015] The synthesis technique of the 1-hydroxycyclohexyl phenyl ketone of the present embodiment comprises the following steps:

[0016] (1) Acylation: Put cyclohexyl formic acid into the reaction kettle, raise the temperature to 35±5°C, add phosphorus trichloride, keep it at 603°C for 3 hours, remove the inorganic layer to obtain cyclohexylcarbonyl chloride; among them, the raw material The weight ratio of cyclohexyl formic acid and phosphorus trichloride is 3.2:1;

[0017] (2) Friedel-Crafts reaction: add benzene and catalyst aluminum trichloride to the reaction kettle, after cooling down to 10°C, add cyclohexanecarbonyl chloride, benzene, aluminum trichloride and cyclohexane The weight ratio of formyl chloride is

[0018] 9:2.9:3.16, at 17°C for 2.5 hours, the complex of cyclohexyl phenyl ketone and aluminum trichloride was obtained;

[0019] (3) Hydrolysis reaction: add an appropriate amount of dilute hydrochloric acid with a mass concentration of 1.5% to the complex, s...

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Abstract

The present invention discloses a 1-hydroxy cyclohexyl phenyl methanone synthesis process, which is characterized in that cyclohexyl formic acid is adopted as a raw material, an acylation reaction, a Friedel-Crafts reaction, and an alkaline hydrolysis reaction are performed to obtain a 1-hydroxy cyclohexyl phenyl methanone crude product, and fine steaming, crystallization, and drying are performed to obtain the 1-hydroxy cyclohexyl phenyl methanone finished product. According to the present invention, the process is reasonable, no sulfur dioxide gas emits during the production process, the environmental pollution caused by the produced sodium chloride is low, and the product yield is high.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a synthesis process of 1-hydroxycyclohexyl phenyl ketone. Background technique [0002] The synthesis process of 1-hydroxycyclohexyl phenyl ketone at least includes processes such as acylation reaction, Friedel-Crafts reaction, and chlorination reaction. In the current synthesis process method of 1-hydroxycyclohexyl phenyl ketone, the technical process is not easy to implement, the resulting 1-hydroxy cyclohexyl phenyl ketone has low purity, the reaction residue cannot be recycled, and the production process is complicated. The production efficiency is low and the cost is high, so it is not suitable for large-scale production. Contents of the invention [0003] In order to overcome the above-mentioned technical problems existing in the prior art field, the object of the present invention is to provide a synthesis process for 1-hydroxycyclohexyl pheny...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/83C07C45/64
Inventor 吕艳
Owner 吕艳