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7-phenylacetylamino-3-chloromethyl cephalosporanic acid p-methoxy benzyl ester powder and preparing process thereof

A technology of chloromethyl cephalosporanic acid and phenylacetamide, which is applied in the field of 7-phenylacetamide-3-chloromethyl cephalosporanic acid p-methoxybenzyl powder and its preparation, and can solve the problem of affecting function and particle size uniformity , poor fluidity and solubility, etc., to achieve the effect of easy dissolution, good fluidity and uniform particle size

Inactive Publication Date: 2004-09-01
HEZE RUIZHI TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the disadvantages of this crystal are that the particle size uniformity, fluidity and solubility are not good, which affects its function.

Method used

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  • 7-phenylacetylamino-3-chloromethyl cephalosporanic acid p-methoxy benzyl ester powder and preparing process thereof
  • 7-phenylacetylamino-3-chloromethyl cephalosporanic acid p-methoxy benzyl ester powder and preparing process thereof
  • 7-phenylacetylamino-3-chloromethyl cephalosporanic acid p-methoxy benzyl ester powder and preparing process thereof

Examples

Experimental program
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Effect test

example 1

[0021] Dissolve 40 grams of GCLE crude product in 250 ml of acetonitrile at 40°C, stir until fully dissolved, concentrate the solvent to about 1 / 2 under reduced pressure, at this time, a large amount of solid precipitates, cool down to 3°C, and stir at this temperature for 1.5 hours, filter , washed with 30 milliliters of dichloromethane at 3°C, and then the solid was dissolved in 200 milliliters of dichloromethane and 40 milliliters of N,N-dimethylformamide mixed solvent at 35°C, and the product 19 was dried with a powder spray dryer grams; drying conditions: inlet temperature 80°C, outlet temperature 45°C, feed pump speed 30 rpm, nozzle speed 50 rpm.

example 2

[0023] 40 grams of GCLE crude product was dissolved in a mixed solvent of 200 milliliters of acetonitrile and 100 milliliters of dichloromethane at 35°C, stirred until fully dissolved, and about 1 / 2 of the solvent was concentrated under reduced pressure. Stir at this temperature for 1.5 hours, filter, wash with 30 ml of 3°C dichloromethane, then dissolve the solid in 200 ml of dichloromethane and 40 ml of N,N-dimethylformamide mixed solvent at 40°C, 20 grams of product dried with a powder spray dryer; drying conditions: inlet temperature 65°C, outlet temperature 48°C, feed pump speed 20 rpm, nozzle speed 50 rpm.

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Abstract

The invention provides a mixed powder of 7-phenylacetamide-3- chloromethyl cephalosporanic acid methoxy benzyl ester (GCLE) non-shaping member and crystal, which has epigranularity, good fluidity, easy dissolution and long-period stabilization under economical storage condition, wherein the preparation method for the mixed powder comprises the steps of, purifying the crude GCLE product through fusion medium to obtain high purity GCLE, then dissolving it in organic fusion medium, and applying powder to the solution. The powder can be used as the synthetic raw material for various cephalosporin.oxysilane

Description

technical field [0001] The invention relates to 7-phenylacetamide-3-chloromethyl cephalosporanic acid p-methoxybenzyl GCLE powder and a preparation method thereof. Background technique [0002] The cephalosporin intermediate represented by the following formula is known as an important compound for the synthesis of various cephalosporins. [0003] [0004] Such as ceftazidime, cefixime and so on. [0005] This compound is conventionally prepared by, for example, the method described in Japanese Patent Publication No. 41153 / 1989, but only an oily substance can be obtained, which is unstable. In recent years, it has been reported to make it into crystal form, which increases its stability. However, the disadvantages of this crystal are poor uniformity in particle size, fluidity, and solubility, which affect its function. Contents of the invention [0006] One of purpose of the present invention is to overcome above-mentioned deficiencies in the prior art, and provide a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/24
Inventor 彭继先杨宇晁明永
Owner HEZE RUIZHI TECH DEV