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1/4 water and cefamandole nafate compound

A technology of cefamandide sodium and montdol sodium, which is applied in the directions of organic chemistry, antibacterial drugs, organic active ingredients, etc., can solve the problems of unqualified turbidity, low thermal decomposition temperature, poor fluidity, etc., and achieve product quality Stable, wide application prospects, good thermal stability

Active Publication Date: 2017-06-13
HAINAN LINGKANG PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In addition, the cefamandole sodium compound prepared by the above method is an anhydrous substance, which has serious problems such as poor storage stability, low thermal decomposition temperature, poor fluidity, and easy moisture absorption.
Thereby affecting the product quality, resulting in unclear preparation products, unqualified turbidity, and reducing the stability of the preparation

Method used

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  • 1/4 water and cefamandole nafate compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] The preparation of embodiment 1 1 / 4 cefamandole sodium compound

[0026] (1) 1L acetonitrile, 200g 3-acetoxymethyl-5-sulfur-7-amino-8-oxo-1-azabicyclooct-2-ene-2carboxylic acid, 1kg methylmercaptotetrazolium, Mix 900ml of boron trifluoride / acetonitrile complex, heat up to 30°C, stir rapidly for 2 hours, cool down to 0°C after the reaction, mix the reaction liquid with 1.5L of purified water pre-cooled to 0°C, and stir slowly until After crystals are precipitated, stir for another 30 minutes, add 10% ammonia water to adjust the pH value to 3.0, control the temperature at 0-5° C., grow the crystals for 2 hours, filter, wash twice with 1 L of acetone, and dry in vacuum to obtain a white crystalline powder (6R ,7R)-7amino-3[(Z)-2-(4-methylthiazol)-5-yl]vinyl-8oxo-5-thia-1-azabicyclo[4.2.0]octane -2-ene-2-carboxylic acid (223.5 g);

[0027] (2) (6R,7R)-7amino-3[(Z)-2-(4-methylthiazol)-5-yl]vinyl-8oxo-5-thia-1-azabicyclo [4.2.0] Mix oct-2-ene-2-carboxylic acid with 2L of e...

Embodiment 2

[0029] The preparation of embodiment 2 1 / 4 cefamandole sodium compound

[0030] (1) Mix 1.5L acetonitrile, 300g 3-acetoxymethyl-5-sulfur-7-amino-8-oxo-1-azabicyclooct-2-ene-2carboxylic acid, 1.5kg methylmercaptotetraazole Mix oxazole and 1.4L boron trifluoride / acetonitrile complex, raise the temperature to 40°C, stir the reaction rapidly for 1h, cool down to 5°C after the reaction, and mix the reaction solution with 2.25L purified water pre-cooled to 5°C, Stir slowly until crystals are precipitated, then stir for 30 minutes, add 10% ammonia water to adjust the pH to 3.4, control the temperature at 0-5°C, grow crystals for 3 hours, filter, wash twice with 1.5L of acetone, and dry in vacuum to obtain white crystals Sexual powder (6R,7R)-7amino-3[(Z)-2-(4-methylthiazol)-5-yl]vinyl-8oxo-5-thia-1-azabicyclo[4.2 .0] Oct-2-ene-2-carboxylic acid (319.6 g);

[0031] (2) (6R,7R)-7amino-3[(Z)-2-(4-methylthiazol)-5-yl]vinyl-8oxo-5-thia-1-azabicyclo [4.2.0] Mix oct-2-ene-2-carboxylic ac...

Embodiment 3

[0033] The preparation of embodiment 3 1 / 4 cefamandole sodium compound

[0034] (1) 1.25L acetonitrile, 250g 3-acetoxymethyl-5-sulfur-7-amino-8-oxo-1-azabicyclooct-2-ene-2 ​​carboxylic acid, 1.25kg methylmercaptotetraazole Mix oxazole and 1.17L boron trifluoride / acetonitrile complex, heat up to 35°C, stir rapidly for 2 hours, cool down to 3°C after the reaction, mix the reaction solution with 1.88L purified water pre-cooled to 2°C, Stir slowly until crystals are precipitated, then stir for 30 minutes, add 10% ammonia water to adjust the pH to 3.2, control the temperature at 0-5°C, grow crystals for 2 hours, filter, wash twice with 1.3L of acetone, and dry in vacuum to obtain white crystals Sexual powder (6R,7R)-7amino-3[(Z)-2-(4-methylthiazol)-5-yl]vinyl-8oxo-5-thia-1-azabicyclo[4.2 .0] Oct-2-ene-2-carboxylic acid (261.1 g);

[0035] (2) (6R,7R)-7amino-3[(Z)-2-(4-methylthiazol)-5-yl]vinyl-8oxo-5-thia-1-azabicyclo [4.2.0] Mix oct-2-ene-2-carboxylic acid with 2.5L ethyl aceta...

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Abstract

The invention discloses a 1 / 4 water and cefamandole nafate compound and a preparation method thereof. Each mole of cefamandole nafate contains 1 / 4 mole of water. The cefamandole nafate compound prepared by the method is low in impurity content, good in stability, good in mobility and low in hygroscopicity, and has a wider application prospect.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering medicine crystallization, and in particular relates to a 1 / 4 cefamandole sodium compound and a preparation method thereof. Background technique [0002] Cefamandole sodium was successfully created in 1972 by U.S. Lilly Company, and it was first listed in the UK in 1978. Cefamandole sodium is also known as formic acid (acyl) benzyl tetrazole cephalosporin sodium, oxybenzyl tetrazole cephalosporin sodium, Cefadoxazole, oxyzole cephalosporin, Pioneer oxybenzazole, cefamandole formate sodium, Pioneer oxybenzazole, etc., are the second-generation semi-synthetic cephalosporins with strong bactericidal effect, and also have the first-generation And some of the advantages of the third-generation cephalosporins, more stable to β-lactamase, broad antibacterial spectrum. [0003] It is reported in the literature that the synthesis of cefamandole sodium mainly contains the following routes: rout...

Claims

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Application Information

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IPC IPC(8): C07D501/36C07D501/06C07D501/12A61K31/546A61P31/04
CPCC07D501/06C07D501/12C07D501/36
Inventor 陶灵刚
Owner HAINAN LINGKANG PHARMA CO LTD
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