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Preparation method for ketoprofen

A technology of ketoprofen and benzoylphenyl, which is applied in the field of preparation of ketoprofen, can solve the problems of complex production process, low yield of finished product, high production cost, etc., and achieve simple production process and low production cost. Low, little pollution effect

Inactive Publication Date: 2015-11-11
ZHEJIANG BOJU NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The production process of the prior art is complicated, the production cost is high, the pollution is large, and its finished product yield is low

Method used

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  • Preparation method for ketoprofen
  • Preparation method for ketoprofen
  • Preparation method for ketoprofen

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Experimental program
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Embodiment 1

[0029] The preparation method of ketoprofen in this embodiment comprises 3-(1-cyanoethyl)methyl benzoate preparation stage, 3-(1-cyanoethyl)benzoic acid preparation stage, 3-(1-cyanoethyl) Base) benzoyl chloride preparation stage, 2-(3-benzoylphenyl) propionitrile preparation stage and ketoprofen stage, concrete steps are as follows:

[0030] 1) 3-(1-cyanoethyl) methyl benzoate preparation stage

[0031] Add methyl 3-cyanomethylbenzoate, dimethyl carbonate, and potassium carbonate with a molar ratio of 3:20:1 into a dry autoclave, and slowly heat up to 180°C under stirring, and control the pressure below 3MPa. After 30 hours of heat preservation, the reaction is completed; the reaction solution is filtered through pressure, washed with water to neutrality, and then excess dimethyl carbonate is removed by distillation, and high vacuum rectification is carried out to obtain methyl 3-(1-cyanoethyl)benzoate;

[0032] 2) 3-(1-cyanoethyl)benzoic acid preparation stage

[0033] Add...

Embodiment 2

[0041] The preparation method of ketoprofen in this embodiment comprises 3-(1-cyanoethyl)methyl benzoate preparation stage, 3-(1-cyanoethyl)benzoic acid preparation stage, 3-(1-cyanoethyl) Base) benzoyl chloride preparation stage, 2-(3-benzoylphenyl) propionitrile preparation stage and ketoprofen stage, concrete steps are as follows:

[0042] 1) 3-(1-cyanoethyl) methyl benzoate preparation stage

[0043] Add methyl 3-cyanomethylbenzoate, dimethyl carbonate, and potassium carbonate with a molar ratio of 1:10:1 into a dry autoclave, and slowly raise the temperature to 130°C under stirring, and control the pressure below 1.5MPa , and the reaction was completed after being incubated for 50 hours; the reaction solution was filtered through press, washed to neutrality, then distilled to remove excess dimethyl carbonate, and high vacuum rectification obtained 3-(1-cyanoethyl) methyl benzoate;

[0044] 2) 3-(1-cyanoethyl)benzoic acid preparation stage

[0045] Add water and 3-(1-cya...

Embodiment 3

[0053] The preparation method of ketoprofen in this embodiment comprises 3-(1-cyanoethyl)methyl benzoate preparation stage, 3-(1-cyanoethyl)benzoic acid preparation stage, 3-(1-cyanoethyl) Base) benzoyl chloride preparation stage, 2-(3-benzoylphenyl) propionitrile preparation stage and ketoprofen stage, concrete steps are as follows:

[0054] 1) 3-(1-cyanoethyl) methyl benzoate preparation stage

[0055] Add methyl 3-cyanomethylbenzoate, dimethyl carbonate, and potassium carbonate with a molar ratio of 2:8:0.01 into a dry autoclave, and slowly heat up to 300°C under stirring, and control the pressure below 6MPa. After 10 hours of heat preservation, the reaction is completed; the reaction solution is filtered through press, washed with water to neutrality, then the excess dimethyl carbonate is removed by distillation, and high vacuum rectification is carried out to obtain methyl 3-(1-cyanoethyl)benzoate;

[0056] 2) 3-(1-cyanoethyl)benzoic acid preparation stage

[0057] Add ...

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Abstract

The invention discloses a preparation method for ketoprofen. The preparation method sequentially comprises the following steps of: a 3-(1-cyanoethyl)methyl benzoate preparation stage, a 3-(1-cyanoethyl)benzoic acid preparation stage, a 3-(1-cyanoethyl)benzoyl chloride preparation stage, a 2-(3-benzoylphenyl)propionitrile preparation stage and a ketoprofen preparation stage. According to the preparation method, 3-cyanomethyl methyl benzoate is taken a main raw material, and finally prepared into a finished product by methylation reaction, hydrolysis reaction, chloroformylation reaction,Friedel-Crafts reaction and hydrolysis reaction; and the finished product is high in purity, and has a yield higher than 90%. Besides, the production process is simple, the production cost is low and the pollution is less.

Description

technical field [0001] The invention relates to the technical field of medicine and chemical industry, in particular to a preparation method of ketoprofen. Background technique [0002] At present, ketoprofen belongs to the new type of non-steroidal anti-inflammatory drugs of aryl propionic acid, which is used to treat various arthritis, joint swelling and pain caused by ankylosing spondylitis, as well as dysmenorrhea, toothache, postoperative pain and cancer pain Therefore, it is favored by experts and scholars at home and abroad, as well as respected by the medical profession and patients. The production process of the prior art is complicated, the production cost is high, the pollution is large, and the finished product yield is low. Contents of the invention [0003] The technical problem to be solved by the present invention is to provide a preparation method of ketoprofen with simple production process, high product purity and high yield in view of the deficiencies ...

Claims

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Application Information

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IPC IPC(8): C07C51/08C07C59/84
CPCC07C253/30C07C51/08
Inventor 龚华银周俊周邦福
Owner ZHEJIANG BOJU NEW MATERIALS CO LTD
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