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3-chloro methyl benzoic acid synthetic method

A technology of chloromethylbenzoic acid and a synthesis method, applied in the field of preparation of organic intermediates, can solve the problems of high safety risk, complicated purification process, low yield and purity of finished products, etc., and achieves high safety, high purity, and synthetic short route effect

Active Publication Date: 2016-03-09
湖北相和精密化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the defects and deficiencies in the preparation method of 3-chloromethylbenzoic acid in the prior art, such as low product yield and purity, complicated purification process and high safety risk, the present invention provides a novel preparation method of 3-chloromethylbenzoic acid , the method is simple and easy to implement, high in safety, high in finished product yield, and the starting material is cheap and easy to obtain, and the 3-chloromethylbenzoic acid prepared by the preparation method has high purity

Method used

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  • 3-chloro methyl benzoic acid synthetic method

Examples

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Effect test

Embodiment 1

[0025] Put 100ml of dichloromethane into the autoclave, add 0.1mol of benzoyl chloride, 0.15mol of paraformaldehyde, 0.05mol of anhydrous zinc chloride, fill with nitrogen to 0.3Mpa, react at 60℃~70℃ for 15h, then cool down to At room temperature, the nitrogen gas was vented, the reaction solution was dropped into 100ml of ice water, stirred for 0.5h, and the layers were statically separated, and the lower organic layer was removed for HPLC (High Performance Liquid Chromatography, high performance liquid chromatography) analysis, the crude product contained benzoic acid 2.4% (percentage by weight) , 91.6% (weight percent) of 3-chloromethylbenzoic acid.

Embodiment 2

[0027] Put 60ml of chloroform into the autoclave, add 0.1mol of benzoyl chloride, 0.10mol of paraformaldehyde, 0.005mol of anhydrous ferric chloride, fill with nitrogen to 0.5Mpa, react at 20℃~25℃ for 10h, then cool down to room temperature , vent the nitrogen, put the reaction solution into 100ml ice water, stir for 0.5h, static layering, take the lower organic layer for HPLC analysis, the crude product contains 3.1% benzoic acid, 90.2% 3-chloromethylbenzoic acid.

Embodiment 3

[0029] Put 50ml of carbon tetrachloride into the autoclave, add 0.1mol of benzoyl chloride, 0.12mol of paraformaldehyde, 0.02mol of anhydrous aluminum trichloride, fill nitrogen to 0.1Mpa, and react at 55°C to 60°C for 20h, then Cool down to room temperature, vent the nitrogen, put the reaction solution into 100ml of ice water, stir for 0.5h, stand still and separate the layers, take the lower organic layer for HPLC analysis, the crude product contains 8.2% benzoic acid and 87.7% 3-chloromethylbenzoic acid.

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Abstract

The present invention relates to a 3-chloro methyl benzoic acid synthetic method, and the specific method is as follows: in zinc chloride, ferric chloride and other Lewis acid catalysts, 3-chloro methyl benzoic acid is synthesized from benzoyl chloride and paraformaldehyde in a solvent in one step. The synthetic method is a one-step reaction, and is simple and easy to control, highly-safe, and high in finished product yield, starting materials are cheap and readily available, the synthetic method is less in waste, the waste can be harmlessly processed, and the synthetic method is clean and environmentally-friendly, and the purity of the 3-chloro methyl benzoic acid prepared by the synthetic method is high.

Description

technical field [0001] The invention relates to a method for preparing an organic intermediate, in particular to a method for synthesizing 3-chloromethylbenzoic acid, and belongs to the technical field of chemical industry. Background technique [0002] 3-Chloromethylbenzoic acid is a very useful intermediate that can be used to synthesize many products, such as ketoprofen. At present, there are not many synthetic methods of 3-chloromethylbenzoic acid recorded in the prior art, and almost all of them start from m-xylene. First, m-xylene is mono-oxidized to generate 3-methylbenzoic acid, 3-methylbenzoic acid Then substituted by photochlorination to obtain 3-chloromethylbenzoic acid. [0003] There are obvious deficiencies and defects in the prior art: one, the single oxidation selectivity of m-xylene is not strong, and two methyl groups will be oxidized simultaneously to form isophthalic acid, which reduces the purity and yield of 3-methylbenzoic acid ; Its di-photochlorina...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/04C07C63/70
CPCC07C51/04C07C63/70
Inventor 易章国殷少华董晓露
Owner 湖北相和精密化学有限公司
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