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A kind of preparation method of aceclofenac

A technology of aceclofenac and acid hydrolysis, which is applied in the field of preparation and purification of aceclofenac, can solve problems such as complex operation, low product yield, and high environmental protection pressure, and achieve the reduction of impurity content, low equipment corrosiveness, The effect of increasing the conversion rate

Active Publication Date: 2021-12-28
LUNAN PHARMA GROUP CORPORATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The object of the present invention is to provide a kind of preparation method of aceclofenac for the environmental protection pressure that exists in the current preparation process of aceclofenac tert-butyl ester acidolysis, complex operation, low product yield etc. The method has mild reaction conditions, simple operation, high process conversion rate, and easy industrial production. The purity of the crude product reaches 97.63%, and the purity of the pure product is up to 99.95%, and the maximum content of the impurity is less than 0.04%.

Method used

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  • A kind of preparation method of aceclofenac

Examples

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Embodiment 1

[0029] The preparation of embodiment 1 aceclofenac

[0030] Add 500g of tert-butyl aceclofenac to a 2L three-necked flask, under stirring, add 500ml of acetic acid, 15ml of concentrated hydrochloric acid solution (mass fraction is 36%), 500ml of acetic anhydride, heat up to 50°C for 4h, cool to 10°C Stir and crystallize at -30°C for 2h, filter with suction, rinse the filter cake with an appropriate amount of purified water, and dry it in vacuum at 50°C for 8h to obtain 419.2g of white solid, which is the crude product of aceclofenac, with a yield of 97.3% and a purity of 99.82% by HPLC. . The maximum single impurity is 0.03% of aceclofenac tert-butyl ester.

[0031] Add 419.2g of crude aceclofenac and 840ml of acetic acid into a 2L three-necked flask, heat until the solid dissolves, add 4.2g of activated carbon after dissolution, keep stirring for 1 hour, then suction filter while it is hot, cool the filtrate to 25°C, stir and crystallize for 4 hours, After suction filtratio...

Embodiment 2

[0032] The preparation of embodiment 2 aceclofenac

[0033] Add 500g of tert-butyl aceclofenac to a 2L three-necked flask, under stirring, add 500ml of acetic acid, 25ml of concentrated hydrochloric acid solution (mass fraction is 37%), 500ml of acetic anhydride, heat up to 60°C for 3h, cool to 10°C Stir and crystallize at -30°C for 2h, filter with suction, rinse the filter cake with an appropriate amount of purified water, and dry in vacuum at 50°C for 8h to obtain 418.3g of white solid, which is aceclofenac, with a yield of 97.1% and a purity of 99.80% by HPLC. The maximum single impurity is 0.04% of aceclofenac tert-butyl ester.

[0034] Add 418.3g of crude aceclofenac and 840ml of acetic acid to a 2L three-necked flask, heat until the solid dissolves, add 8.4g of activated carbon after dissolution, keep stirring for 1 hour, then suction filter while it is hot, cool the filtrate to 25°C, stir and crystallize for 4 hours, After suction filtration, the filter cake was rinsed...

Embodiment 3

[0035] The preparation of embodiment 3 aceclofenac

[0036] Add 500g of aceclofenac tert-butyl ester to a 5L three-necked flask, under stirring, add 1500ml of formic acid, 100ml of concentrated hydrochloric acid solution (mass fraction is 38%), 850ml of acetic anhydride, heat up to 50°C for 6h, cool to 10°C Stir and crystallize at -30°C for 2 hours, filter with suction, rinse the filter cake with an appropriate amount of purified water, and dry it in vacuum at 50°C for 8 hours to obtain 417.0 g of white solid, which is the crude product of aceclofenac. The yield is 96.8%, and the HPLC purity is 99.71%. . The maximum single impurity is 0.07% of aceclofenac tert-butyl ester.

[0037] Add 417.0g of crude aceclofenac and 840ml of formic acid to a 2L three-necked flask, heat until the solid dissolves, add 8.4g of activated carbon after dissolution, keep stirring for 1 hour, then suction filter while it is hot, cool the filtrate to 25°C, stir and crystallize for 4 hours, After suc...

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Abstract

The invention belongs to the technical field of medicine, and in particular relates to a preparation method of aceclofenac. The method of the present invention takes aceclofenac tert-butyl as starting material, acidolysis obtains aceclofenac crude product in the mixed solvent of low-molecular organic acid, hydrogen halide aqueous solution and low-molecular organic acid anhydride; Then aceclofenac The crude acid is refined in low-molecular organic acid to obtain the refined product of aceclofenac. The method provided by the invention can significantly improve the yield and purity of aceclofenac, is easy to operate, improves production efficiency, and is more suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of medicine synthesis, and in particular relates to a method for preparing and purifying aceclofenac. Background technique [0002] The compound involved in the present invention is 2-(2,6-dichloroanilino) phenylacetoxyacetic acid, and the specific structural formula is as follows: [0003] [0004] Aceclofenac, namely 2-(2,6-dichloroanilino)phenylacetoxyacetic acid, is a new non-steroidal anti-inflammatory drug with good safety. It was developed by Almirall-Prodespharm Pharmaceutical Company of Spain and first listed in Spain in 1992. It was listed in European Pharmacopoeia and British Pharmacopoeia in 1998 and has been listed in more than 20 countries including Britain, Germany, France and Spain. It is clinically used to relieve inflammation and pain caused by rheumatoid arthritis, rheumatoid arthritis and ankylosing spondylitis, and is a safe and reliable drug for treating acute and chronic pain and a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C229/42C07C227/16C07C227/42
CPCC07C227/16C07C227/42C07C229/42
Inventor 王永珍鲍广龙
Owner LUNAN PHARMA GROUP CORPORATION
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