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Synthesis method of diclofenac sodium

A technology of diclofenac sodium and a synthesis method, applied in the field of diclofenac sodium synthesis, can solve the problems of unobtainable raw materials, three-waste pollution, and high cost, and achieve the effects of facilitating subsequent treatment, reducing the generation of by-products, and improving yields

Pending Publication Date: 2021-09-17
HENAN KANGDA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese scholars have also improved this method, but the yield is still generally low, and the raw materials are not easy to obtain, the cost is high, and the pollution of the three wastes is serious

Method used

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  • Synthesis method of diclofenac sodium

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] A kind of synthetic method of diclofenac sodium, comprises the following steps:

[0034](1) Put 2 parts of toluene, 0.5 parts of aniline and 0.005 parts of benzyltriethylammonium chloride into a dry four-necked bottle, start the tail gas absorption, stir and drop 0.6 parts of chloroacetyl chloride in the solution, drop The time is about 1.5h, the temperature is controlled at 15°C, and the temperature is slowly raised to 80°C after dropping, and a small amount of toluene is added after 4 hours of reflux and heat preservation, and the temperature is lowered to 60°C. Then add 1 part of 2,6-dichlorophenol and 0.6 part of sodium carbonate, heat up to 80°C, keep warm for 18h and then cool to 75°C. Add purified water, raise the temperature to 80°C, continue to stir and keep warm for 1h, let stand, extract the oil layer, add 0.4 parts of triethylamine, keep warm at 80°C for 6h. Wash with water, separate the oil layer, distill under normal pressure and then under reduced pressu...

Embodiment 2

[0039] (1) Put 8 parts of toluene, 0.8 parts of aniline and 0.5 parts of tetrabutylammonium bromide into a dry four-necked bottle, start the tail gas absorption, stir and drop 1.0 parts of chloroacetyl chloride in the solution, and the dropping time is About 1.5h, the temperature is controlled at 25°C, and the temperature is slowly raised to 100°C after dropping, and a small amount of toluene is added after reflux for 4 hours, and the temperature is lowered to 70°C. Then add 1 part of 2,6-dichlorophenol and 0.6 part of sodium carbonate, raise the temperature to 120°C, keep it warm for 18 hours and then cool to 75°C. Add purified water, raise the temperature to 100°C, continue to stir and keep warm for 1h, let it stand still, extract the oil layer, add 2.0 parts of sodium methoxide, raise the temperature to 110°C and keep warm for 6h. Wash with water, separate the oil layer, distill under normal pressure and then under reduced pressure, recover toluene, and collect fractions at...

Embodiment 3

[0044] (1) Put 5 parts of toluene, 0.6 parts of aniline and 0.25 parts of catalyst into a dry four-necked bottle. The catalysts are tetrabutylammonium chloride and tetrabutylammonium bisulfate. Turn on the tail gas absorption, stir and drop in the solution Add 0.8 parts of chloroacetyl chloride for about 1.5 hours, control the temperature at 20°C, slowly raise the temperature to 90°C after dropping, add a small amount of toluene after reflux for 4 hours, and cool down to 65°C. Then add 1 part of 2,6-dichlorophenol and 0.6 part of sodium carbonate, heat up to 100°C, keep warm for 18h and then cool to 75°C. Add purified water, raise the temperature to 90°C, continue to stir and keep warm for 1h, let stand, extract the oil layer, add 1.2 parts of sodium ethoxide and tert-butanol, keep warm at 95°C for 6h. Wash with water, separate the oil layer, distill under normal pressure and then under reduced pressure, recover toluene, and collect fractions at 180-260°C through reduced-press...

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Abstract

The invention discloses a synthesis method of diclofenac sodium, which comprises the following steps: (1) dropwise adding chloroacetyl chloride into toluene, aniline and a catalyst solution while stirring, carrying out heat preservation reflux, then adding 2, 6-dichlorophenol and sodium carbonate, carrying out heat preservation reflux, extracting with water to obtain an oil layer, adding alkali into the oil layer, and carrying out heat preservation reaction to obtain 2, 6-dichlorodiphenylamine; (2) heating and melting the 2, 6-dichlorodiphenylamine prepared in the step (1), dropwise adding chloroacetyl chloride, heating, carrying out heat preservation reaction, hydrolyzing, and crystallizing to obtain N-(2, 6-dichlorophenyl)-phenyl-chloroacetamide; (3) carrying out heating reaction on the N-(2, 6-dichlorophenyl)-phenyl-chloroacetamide prepared in the step (2) and aluminum trichloride, and carrying out pumping to obtain solid 1-(2, 6-dichlorophenyl)-2-indolinone; and (4) adding the 1-(2, 6-dichlorophenyl)-2-indolinone prepared in the step (3) into alkali liquor, stirring, heating and refluxing to obtain the diclofenac sodium. The synthesis method is stable, easy to operate, low in cost, high in yield and suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of diclofenac sodium synthesis, in particular to a synthesis method of diclofenac sodium. Background technique [0002] Diclofenac sodium (diclofenac), chemical name: 2-[(2,6-dichlorophenyl)amino]-sodium phenylacetate, developed by Ciba-Geigy Ltd. in Switzerland and launched in 1974 A third-generation potent anti-inflammatory analgesic non-steroidal anti-inflammatory drug. It is clinically used to treat various rheumatoid and osteoarthritis, and relieve pain from surgery, strain and trauma. Its effect is 2 to 2.5 times stronger than indomethacin and 26 to 50 times stronger than aspirin. It has significant analgesic, anti-inflammatory, anti-rheumatic and antipyretic effects, no obvious side effects, good tolerance, and rapid oral absorption. [0003] Non-steroidal anti-inflammatory drugs (NSAIDs) are the fastest growing drugs in the world. Since the side effects of coxib drugs were exposed one after anoth...

Claims

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Application Information

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IPC IPC(8): C07C227/22C07C229/42C07D209/34C07C233/15C07C209/60C07C211/56C07C231/02C07C233/07
CPCC07C227/22C07D209/34C07C209/60C07C231/02C07C233/07C07C211/56C07C233/15C07C229/42
Inventor 李文杰孔芹芹罗礼帅郭琦周从旭白金钟曹文英张君郭贺威王洋洋王中华
Owner HENAN KANGDA PHARMA
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