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A kind of preparation method of the butoconazole nitrate intermediate suitable for industrialized production

A technology for butoconazole nitrate and intermediates, which is applied in the field of preparation of butoconazole nitrate intermediates, can solve the problems of personnel damage and equipment damage, difficult control of Grignard reaction, ether volatilization, etc., so as to reduce side reactions and increase operability Sexuality and safety, the effect of increasing feasibility

Active Publication Date: 2015-12-23
SHANDONG ACADEMY OF PHARMACEUTICAL SCIENCES
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Problems solved by technology

Using part of the ether for the reaction will also cause the Grignard reaction to be difficult to control, especially in large-scale industrial production, which will cause a large amount of ether to volatilize, even cause an explosion, and cause damage to personnel and equipment.

Method used

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  • A kind of preparation method of the butoconazole nitrate intermediate suitable for industrialized production
  • A kind of preparation method of the butoconazole nitrate intermediate suitable for industrialized production
  • A kind of preparation method of the butoconazole nitrate intermediate suitable for industrialized production

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Embodiment 1

[0031] 1. Grignard reaction: In a 20L dry reaction kettle, add 504g (21mol) of magnesium powder, 6.4L of anhydrous methyl tert-butyl ether and tetrahydrofuran (volume ratio 15:1) mixed solvent and a catalytic amount of iodine in sequence at room temperature , under stirring, first drop 0.6-0.8L of anhydrous methyl tert-butyl ether solution (4L in total) containing 3.22kg (20mol) of p-chlorobenzyl chloride, and stir until the reaction is initiated (the solution becomes cloudy and the temperature rises), and the temperature Raise to about 40°C, continue to add the remaining solution, keep at 40-50°C, drop for about 1-2 hours, and keep warm for 1-2 hours.

[0032] 2. Condensation reaction: the above reaction system is lowered to room temperature, and directly dropwise add 1.85kg (20mol) of epichlorohydrin 4L solution of anhydrous methyl tert-butyl ether to the reaction kettle under stirring, control the dropping rate and maintain the temperature At about 40°C, drop it in about 1 ...

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Abstract

The invention provides a method for industrial production of a butoconazole nitrate intermediate, that is 1-chloro-4-p-chlorophenyl-2-butanol (a compound in formula II). The method of the invention comprises: 1. a Grignard reaction, that is, adopting p-chlorobenzyl chloride as a raw material, and performing a Grignard reaction with magnesium powder in a mixed solvent of methyl tertiary butyl ether and tetrahydrofuran; 2. a condensation reaction, that is, continuing reaction by adding epichlorohydrin to obtain the compound II which is an important intermediate for preparing butoconazole nitrate. According to the method, the raw materials are cheap and easily available, the reaction solvent is safer, and the method is suitable for industrial production.

Description

technical field [0001] The present invention relates to the field of organic chemistry and pharmaceutical chemistry, specifically, the present invention relates to a kind of preparation method of butoconazole nitrate intermediate (formula II compound) suitable for industrialized production. Background technique [0002] Butoconazole Nitrate (ButoconazoleNitrate, 64872-76-0), chemical name 1-[4-(4-chlorophenyl)-2-[(2,6-dichlorophenyl)thio]butyl]-1H -Imidazole nitrate, (±)-1-[4-(4-chlorophenyl)-2-[(2,6-dichlorophenyl)thio]butyl]-1H-imidazolemononitrate, is a novel broad-spectrum imidazole antifungal The drug mainly acts on the fungal cell membrane, which increases its osmotic resistance and reduces the fungal viability by changing the permeability of the cell membrane. It is highly effective against vaginal infections caused by Candida albicans, Candida tropicalis and other species of this genus. It is used for vulva and vaginal fungal infections caused by Candida after diagn...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C33/46C07C29/64
CPCC07C29/64C07F3/02C07C33/46
Inventor 郑德强王长斌赵国敏毋立华刘文涛孙利民任文杰李帅索栋
Owner SHANDONG ACADEMY OF PHARMACEUTICAL SCIENCES
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