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Recrystallization method of sertaconazole nitrate

A technology of sertaconazole nitrate and recrystallization, applied in the direction of organic chemistry, etc., can solve problems such as different melting points

Pending Publication Date: 2021-12-21
HAINAN HAISHEN TONGZHOU PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the melting point of sertaconazole nitrate recorded in the European Pharmacopoeia or the British Pharmacopoeia is 156-161°C, which is obviously different from the melting point recorded in the Chinese drug standards

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Drying the crude product of sertaconazole nitrate until the moisture content is below 1%;

[0037] Add 60.63 g of 95% ethanol into the reaction bottle, stir, heat, and raise the temperature to 60° C., add 23.04 g of dried sertaconazole nitrate crude product while stirring, and heat up and reflux for 1 hour. After the heating was stopped, 60.63 g of purified water was added dropwise with stirring, and crystals were precipitated. After the dropwise addition was completed, the mixture was stirred for another 30 minutes and filtered to obtain crystals. Dry in a vacuum oven to obtain the finished product of sertaconazole nitrate. It has been determined that the melting point of the finished product of sertaconazole nitrate is 158.2-159.0°C.

Embodiment 2

[0039] Drying the crude product of sertaconazole nitrate until the moisture content is below 1%;

[0040] Add 100 g of 95% ethanol into the reaction bottle, stir, heat, and raise the temperature to 60° C., add 23.04 g of dried sertaconazole nitrate crude product while stirring, and heat up and reflux for 1 hour. After the heating was stopped, 60.63 g of purified water was added dropwise with stirring, and crystals were precipitated. After the dropwise addition was completed, the mixture was stirred for another 30 minutes and filtered to obtain crystals. Dry in a vacuum oven to obtain the finished product of sertaconazole nitrate. It has been determined that the melting point of the finished product of sertaconazole nitrate is 158.8-159.6°C.

Embodiment 3

[0042] Drying the crude product of sertaconazole nitrate until the moisture content is below 1%;

[0043] Add 60.63 g of 95% ethanol into the reaction bottle, stir, heat, and raise the temperature to 60° C., add 23.04 g of dried sertaconazole nitrate crude product while stirring, and heat up and reflux for 1 hour. After the heating was stopped, 100 g of purified water was added dropwise with stirring, and crystals were precipitated. After the dropwise addition was completed, the mixture was stirred for 30 minutes, and filtered to obtain crystals. Dry in a vacuum oven to obtain the finished product of sertaconazole nitrate. It has been determined that the melting point of the finished product of sertaconazole nitrate is 159.0-159.8°C.

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Abstract

The invention discloses a recrystallization method of sertaconazole nitrate. The recrystallization method is used for preparing a sertaconazole nitrate bulk drug with a melting point of 156-161 DEG C. The recrystallization method comprises the following steps: (1) drying a sertaconazole nitrate crude product until the moisture content is 1% or below; (2) mixing the sertaconazole nitrate crude product with ethanol with the concentration of 90-100%, and heating to reflux; (3) after refluxing for 1-2 hours, dropwise adding water into the mixed solution while stirring, and separating out crystals; and (4) after dropwise adding, filtering and drying the crystal. According to the method, a sertaconazole nitrate bulk drug with the melting point of 156-161 DEG C can be obtained. The melting point of the raw material medicine meets the requirements of European Union Pharmacopoeia or British Pharmacopoeia, and technical support is provided for exporting the medicine to the countries and regions.

Description

technical field [0001] The invention relates to the technical field of preparation of raw materials, in particular to a recrystallization method of sertaconazole nitrate. Background technique [0002] Sertaconazole nitrate is a synthetic imidazole broad-spectrum antifungal drug, which can inhibit and kill dermatophytes, yeasts, candida, and aspergillus, and has strong antibacterial effects on Gram-positive bacteria. [0003] For the purification of sertaconazole nitrate crude drug, the prior art generally adopts 95% ethanol to heat and dissolve the crude sertaconazole nitrate, then cool down and stand for crystallization to recrystallize it. The inventors found that by adopting this recrystallization method, the melting point of the obtained sertaconazole nitrate is 163-167° C., which meets the requirements of the National Drug Standards of the State Food and Drug Administration of China. [0004] However, the melting point of sertaconazole nitrate recorded in the European ...

Claims

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Application Information

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IPC IPC(8): C07D409/12
CPCC07D409/12
Inventor 韦家华李博福
Owner HAINAN HAISHEN TONGZHOU PHARM CO LTD
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