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New crystal form cefmenoxine hydrochloride compound prepared by adopting particle process crystal product molecular assembling and morphology optimizing technology and preparation

A technology of cefmenoxime hydrochloride and its compound, applied in the field of medicine, can solve problems such as poor color grade, poor stability of conventional crystal form of cefmenoxime hydrochloride, and occurrence of degradation products

Inactive Publication Date: 2016-05-11
HAINAN LINGKANG PHARMA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Adopt the cefmenoxime hydrochloride prepared by said method on the market at present, its purity is relatively poor, color grade is bad, poor stability, thereby has influenced its preparation quality
[0006] The conventional crystal form of cefmenoxime hydrochloride has poor stability, and is unstable to heat, acidic environment, and alkaline environment. It is manifested in problems such as easy discoloration of appearance, decrease in content, and occurrence of degradation products.

Method used

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  • New crystal form cefmenoxine hydrochloride compound prepared by adopting particle process crystal product molecular assembling and morphology optimizing technology and preparation
  • New crystal form cefmenoxine hydrochloride compound prepared by adopting particle process crystal product molecular assembling and morphology optimizing technology and preparation
  • New crystal form cefmenoxine hydrochloride compound prepared by adopting particle process crystal product molecular assembling and morphology optimizing technology and preparation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment 1: Preparation of Cefmenoxime Hydrochloride New Crystal Form Compound

[0024] (1) Add 250ml of dichloromethane, 25ml of ethanol, (6R,7R)-7-amino-3-[[(1-methyl-1-H-tetrazol-5-yl)sulfur into the reaction bottle Substitute]methyl]-8-oxo-5-thia·1-azabicyclo[4,2,0]oct-2-ene-2-carboxylate hydrochloride (7-ATCA·HCl) 25g, 20ml of triethylamine, after reacting at room temperature for 30min, add 50.0g of 2-(2-amino-4-thiazolyl)-2-(methoxyimino)acetic acid thiobenzothiazolyl ester (AE active ester), and control the appropriate React at temperature for 8 hours, add water to extract twice, 150ml each time, combine the water phases, decolorize with activated carbon at room temperature, filter, wash the carbon layer with ethanol, combine the washings, adjust the pH value to 1.5 with 6mol / L hydrochloric acid, grow crystals for 3 hours, filter , washed the filtrate with water, and dried under vacuum at 40°C to obtain crude cefmenoxime hydrochloride.

[0025] (2) Add 25.9 g...

Embodiment 2

[0032] Embodiment 2: Preparation of new crystal form compound of cefmenoxime hydrochloride

[0033] (1) Add 250ml of dichloromethane, 25ml of ethanol, (6R,7R)-7-amino-3-[[(1-methyl-1-H-tetrazol-5-yl)sulfur into the reaction bottle Substitute]methyl]-8-oxo-5-thia·1-azabicyclo[4,2,0]oct-2-ene-2-carboxylate hydrochloride (7-ATCA·HCl) 25g, 20ml of triethylamine, after reacting at room temperature for 30min, add 25.0g of 2-(2-amino-4-thiazolyl)-2-(methoxyimino)acetic acid thiobenzothiazolyl ester (AE active ester), and control the appropriate React at temperature for 8 hours, add water to extract twice, 150ml each time, combine the water phases, decolorize with activated carbon at room temperature, filter, wash the carbon layer with ethanol, combine the washings, adjust the pH value to 2.0 with 8mol / L hydrochloric acid, grow crystals for 3 hours, filter , washed the filtrate with water, and dried under vacuum at 40°C to obtain crude cefmenoxime hydrochloride.

[0034] (2) Add 25....

Embodiment 3

[0036]Embodiment 3: Preparation of new crystal form compound of cefmenoxime hydrochloride

[0037] (1) Add 250ml of dichloromethane, 25ml of ethanol, (6R,7R)-7-amino-3-[[(1-methyl-1-H-tetrazol-5-yl)sulfur into the reaction bottle Substitute]methyl]-8-oxo-5-thia·1-azabicyclo[4,2,0]oct-2-ene-2-carboxylate hydrochloride (7-ATCA·HCl) 25g, 20ml of triethylamine, after reacting at room temperature for 30min, add 75.0g of 2-(2-amino-4-thiazolyl)-2-(methoxyimino)acetic acid thiobenzothiazolyl ester (AE active ester) to control the appropriate React at temperature for 8 hours, add water to extract twice, 150ml each time, combine the water phases, decolorize with activated carbon at room temperature, filter, wash the carbon layer with ethanol, combine the washings, adjust the pH value to 2.0 with 5mol / L hydrochloric acid, grow crystals for 3 hours, filter , washed the filtrate with water, and dried under vacuum at 40°C to obtain crude cefmenoxime hydrochloride.

[0038] (2) Add 23.7 g...

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Abstract

The invention discloses a new crystal form cefmenoxine hydrochloride compound and a crystallization preparation method thereof. The new crystal form cefmenoxine hydrochloride compound is prepared by adopting the particle process crystal product molecular assembling and morphology optimizing technology. The compound has the advantages of being high in purity and good in fluidity and stability. The invention also discloses a preparation which is prepared from the cefmenoxine hydrochloride compound, namely cefmenoxine hydrochloride for injection.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a new crystal form compound of cefmenoxime hydrochloride and a preparation using particle process crystal product molecular assembly and shape optimization technology. Background technique [0002] Cefmenoxime hydrochloride, its chemical name is: (6R, 7R)-7-[(Z)-2-(2-amino-4-thiazolyl)-2-methoxyiminoacetamido]-3-[[ 1-Methyl-1H-tetrazol-5-yl)-thio]methyl]-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-metha Hydrochloride (2:1), molecular formula: C 16 h 17 N 9 o 5 S 3 1 / 2HC1, molecular weight: 529.79, structural formula: [0003] [0004] Cefmenoxime hydrochloride is the third-generation cephalosporin developed by Takeda Corporation of Japan. It was first listed in Japan in 1983. It is a broad-spectrum antibiotic that achieves bactericidal effect by inhibiting the biosynthesis of bacterial cell walls. [0005] Regarding the synthetic method of cefmenoxime hydro...

Claims

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Application Information

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IPC IPC(8): C07D501/36C07D501/06C07D501/12A61K31/546A61P31/04
CPCA61K31/546C07D501/06C07D501/12C07D501/36C07B2200/13
Inventor 陶灵刚王静康尹秋响郝红勋
Owner HAINAN LINGKANG PHARMA CO LTD
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