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Preparation method of butoconazole nitrate

A technology of butoconazole nitrate and imidazole, which is applied in the field of preparation of butoconazole nitrate, can solve the problems of complex preparation method, low product purity, and low recovery rate of butoconazole nitrate, and achieve low cost, high product purity and simple steps simple effect

Inactive Publication Date: 2017-12-22
JIANGXI YONGTONG TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The existing butoconazole nitrate preparation method is complicated, the recovery rate is low, and the product purity is low

Method used

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  • Preparation method of butoconazole nitrate
  • Preparation method of butoconazole nitrate
  • Preparation method of butoconazole nitrate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] A preparation method of butoconazole nitrate, which comprises the following steps:

[0035] (1) Synthesis of 1-chloro-4-(4-chlorophenyl)-2-butanol, adding magnesium powder and anhydrous ether in the reaction flask, the mass ratio of magnesium powder and anhydrous ether is 12:142.7, Then add 4-chlorobenzyl chloride and anhydrous ether in the dropping funnel to obtain a mixed solution, the mass ratio of magnesium powder to 4-chlorobenzyl chloride and anhydrous ether in the mixed solution is 12:80:114.1, and add to the reaction flask Add the mixed solution in the reaction bottle, the volume ratio of the added mixed solution to the anhydrous ether in the reaction bottle is 2.5:200, the surface gas of the magnesium powder is generated, the solution is turbid and there is ether reflux, start stirring, and slowly add the rest of the mixed solution dropwise, Control the rate of addition, keep the diethyl ether solution in a slightly boiling state, reflux for 18 minutes after th...

Embodiment 2

[0044] A preparation method of butoconazole nitrate, which comprises the following steps:

[0045] (1) Synthesis of 1-chloro-4-(4-chlorophenyl)-2-butanol, adding magnesium powder and anhydrous ether in the reaction flask, the mass ratio of magnesium powder and anhydrous ether is 12:142.7, Then add 4-chlorobenzyl chloride and anhydrous ether in the dropping funnel to obtain a mixed solution, the mass ratio of magnesium powder to 4-chlorobenzyl chloride and anhydrous ether in the mixed solution is 12:80:114.1, and add to the reaction flask Add the mixed solution in the reaction bottle, the volume ratio of the added mixed solution to the anhydrous ether in the reaction bottle is 2.7:200, the surface gas of the magnesium powder is generated, the solution is turbid and there is ether reflux, start stirring, and slowly add the rest of the mixed solution dropwise, Control the rate of addition, keep the diethyl ether solution in a slightly boiling state, reflux for 18 minutes after th...

Embodiment 3

[0054] A preparation method of butoconazole nitrate, which comprises the following steps:

[0055] (1) Synthesis of 1-chloro-4-(4-chlorophenyl)-2-butanol, adding magnesium powder and anhydrous ether in the reaction flask, the mass ratio of magnesium powder and anhydrous ether is 12:142.7, Then add 4-chlorobenzyl chloride and anhydrous ether in the dropping funnel to obtain a mixed solution, the mass ratio of magnesium powder to 4-chlorobenzyl chloride and anhydrous ether in the mixed solution is 12:80:114.1, and add to the reaction flask Add the mixed solution in the reaction bottle, the volume ratio of the added mixed solution to the anhydrous ether in the reaction bottle is 2.5:200, the surface gas of the magnesium powder is generated, the solution is turbid and there is ether reflux, start stirring, and slowly add the rest of the mixed solution dropwise, Control the rate of addition, keep the ether solution in a slightly boiling state, reflux for 16 minutes after the additi...

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Abstract

The invention discloses a preparation method of butoconazole nitrate. The preparation method comprises the following steps: with 4-chlorobenzyl chloride as a starting raw material, synthesizing 1-chloro-4-(4-chlorophenyl)-2-butanol, then synthesizing 1-(4-(4-chlorophenyl)-2-hydroxy-butyl) imidazole, then synthesizing 1-(4-(4-chlorophenyl)-2-chloro-butyl) imidazole, adding the 1-(4-(4-chlorophenyl)-2-chloro-butyl) imidazole, 2, 6-dichlorobenzenethiol and potassium carbonate into acetone, heating for refluxing, adding water and ethyl acetate after the completion of a reaction, performing liquid separation, sequentially washing an ethyl acetate phase by using saturated potassium carbonate and saturated salt water, drying by using anhydrous magnesium sulfate, removing magnesium sulfate, dropwise adding nitric acid with the concentration of 65% in an ice bath until no precipitate is produced, filtering for collecting solid, and recrystallizing by using absolute ethanol to obtain white crystals, namely the butoconazole nitrate. By the preparation method of the butoconazole nitrate, the process is simple, the yield is high, the cost is low, and the purity of the obtained product is high.

Description

technical field [0001] The invention relates to a preparation method of butoconazole nitrate, which belongs to the technical field of medicine preparation. Background technique [0002] Butoconazole nitrate is an imidazole derivative with antifungal activity, and butoconazole nitrate is an imidazole antifungal drug, which is mainly used for the treatment of vaginal candidiasis. Butoconazole nitrate was first launched in the United States in 1985, and then in Switzerland and France in 1987 and 1988, respectively. [0003] Chinese alias: 1-[4-(4-chlorophenyl)-2-(2,6-dichlorophenyl)thiobutyl]imidazole nitrate, this product is white to off-white crystalline powder, slightly soluble In methanol, slightly soluble in chloroform, dichloromethane, acetone, ethanol, very slightly soluble in ethyl acetate, almost insoluble in water. The melting point is about 159° (decomposition). [0004] The existing butoconazole nitrate preparation method is complicated, the recovery rate is low,...

Claims

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Application Information

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IPC IPC(8): C07D233/60
CPCC07D233/60
Inventor 刘忠春
Owner JIANGXI YONGTONG TECH
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