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Synthesis method of Sertaconazole nitrate

A technology of sertaconazole nitrate and synthesis method, applied in directions such as organic chemistry, can solve the problems of low yield and low purity, and achieve the effects of high yield, high purity and simplified steps

Inactive Publication Date: 2015-08-26
CHIZHOU ZHONGRUI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Low yield, low purity

Method used

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  • Synthesis method of Sertaconazole nitrate

Examples

Experimental program
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Effect test

Embodiment 1

[0017] Weigh 23g of 2-chloro-1-(2,4'-dichlorophenyl)-ethanol into 20mL DMF, stir and mix evenly to obtain 2-chloro-1-(2,4'-dichlorophenyl )-ethanol in DMF;

[0018] Measure DMF: 80mL, imidazole: 8.2g, caustic soda: 8g, PEG600: 1.8g into a four-neck flask, connect a stirrer, thermometer, condensing reflux tube, stir, heat, and slowly raise the temperature to 110°C-115°C , keep warm for 1 hour, cool down to 50°C-55°C; add dropwise 2-chloro-1-(2,4'-dichlorophenyl)-ethanol DMF mixed solution, stir while adding, and control the temperature at 50°C- 55°C, after the dropwise addition, keep warm for 1 hour, then raise the temperature to 110°C-115°C, keep the temperature for 4 hours, and cool down to 60°C after the reaction; continue to put 8g of caustic soda into the reaction device, keep the temperature at 60°C, and stir For 1 hour, add a DMF solution of 2-chloro-3-chloromethylthiophene (31 g of 2-chloro-3-chloromethylthiophene: 80 mL of DMF) dropwise, stirring while adding, and con...

Embodiment 2

[0021] Weigh 23g of 2-chloro-1-(2,4'-dichlorophenyl)-ethanol into 20mL DMF, stir and mix evenly to obtain 2-chloro-1-(2,4'-dichlorophenyl )-ethanol in DMF;

[0022] Measure DMF: 80mL, imidazole: 8.2g, caustic soda: 8g, PEG600: 1.8g into a four-neck flask, connect a stirrer, thermometer, condensing reflux tube, stir, heat, and slowly raise the temperature to 110°C-115°C , keep warm for 1 hour, lower the temperature to 50°C-55°C; add dropwise the DMF solution of 2-chloro-1-(2,4'-dichlorophenyl)-ethanol, stir while adding, and control the temperature at 50°C- 55°C, after the dropwise addition, keep warm for 1 hour, then raise the temperature to 110°C-115°C, keep the temperature for 4 hours, and cool down to 60°C after the reaction; continue to put 8g of caustic soda into the reaction device, keep the temperature at 60°C, and stir For 1 hour, add a DMF solution of 2-chloro-3-chloromethylthiophene (31 g of 2-chloro-3-chloromethylthiophene: 80 mL of DMF) dropwise, stirring while ad...

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PUM

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Abstract

The invention discloses a synthesis method of Sertaconazole nitrate. The method comprises steps as follows: DMF (dimethylformamide), imidazole and caustic soda flakes are added to a reaction container, evenly mixed, slowly heated to the temperature of 110-115 DEG C, kept at the temperature for 1 h and then cooled to the temperature of 50-55 DEG C; a DMF solution of 2-chloro-1-(2,4'-dichlorophenyl)-ethyl alcohol is dropwise added, the temperature is controlled to range from 50 DEG C to 55 DEG C and kept for 1 h after addition, the mixture is heated to the temperature of 110-115 DEG C and kept at the temperature for 4 h, caustic soda flakes are added, a DMF solution of 2-chloro-3-chloromethyl thiophene is dropwise added, the temperature is controlled to range from 50 DEG C to 55 DEG C and kept for 1 h, the mixture is heated to the temperature of 110-115 DEG C for a reaction for 3 h in the temperature range, water is added, and the mixture is cooled to the room temperature; nitric acid is added for acidification, centrifugal filtration is performed, and a crude Sertaconazole nitrate product is obtained through centrifugal filtration; the crude product is dried and recrystallized with methylbenzene, and a dry product is obtained. According to the method, used equipment is simple, steps are simplified, the production cost is low, and the method is suitable for industrial production.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a synthesis method of sertaconazole nitrate. Background technique [0002] Sertaconazole nitrate: Sertaconazole nitrate ointment is a synthetic imidazole broad-spectrum antifungal drug, which can inhibit and kill skin fungi, yeast, Candida, and Aspergillus, and is effective against Gram-positive bacteria. Strong antibacterial effect. [0003] The common synthesis process is: using 2-chloro-1-(2,4'-dichlorophenyl)-ethanol and 3-bromomethyl-7-chlorobenzothiophene as raw materials, in the mixture of isopropanol and organic solvent In the mixed solution, add alkali, react, and then obtain salt through nitric acid, and the organic solvent is toluene, cycloethane or tetrahydrofuran. The yield is low and the purity is not high. Contents of the invention [0004] The purpose of the invention is to provide a synthetic method of sertaconazole nitrate, which has simple equipment, conve...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D409/12
CPCC07D409/12
Inventor 孙建国钱叶发汪千琪朱新民
Owner CHIZHOU ZHONGRUI CHEM
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