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Refining method of cefbuperazone intermediate

A refining method and a technology for intermediates, applied in the field of preparation of cefbuperazone intermediates, can solve the problems of increased preparation costs, high requirements for product preparation scale, increased large-scale production, etc., and meet the requirements of equipment and preparation conditions. High, high preparation purity, simple operation method

Active Publication Date: 2012-04-11
NANJING HAILING TRADITIONAL CHINESE MEDICINE RES CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0015] The shortcoming of said method is, cefbuperazone sodium is the medicine (1.0 gram / support) that uses dosage bigger, therefore very high for the preparation scale requirement of product
However, the preparation of the important intermediate of the product by column chromatography will inevitably increase the difficulty of large-scale production and greatly increase the preparation cost

Method used

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  • Refining method of cefbuperazone intermediate
  • Refining method of cefbuperazone intermediate
  • Refining method of cefbuperazone intermediate

Examples

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Embodiment 1

[0035] The preparation of embodiment 1 formula I intermediate

[0036] According to the method described in Example 4 of the patent "GB2048241": 200 grams of cefbuperazone's 7-position side chain was dissolved in 700 milliliters of anhydrous methylene chloride, and under ice-cooling, 100 grams of oxalyl chloride and 30 milliliters of anhydrous "N , N-dimethylformamide", reacted at room temperature for 30 minutes. After the reaction was completed, the solvent was evaporated to dryness under reduced pressure, 800 ml of anhydrous dichloromethane was added to the residue, the temperature was lowered to -50°C under nitrogen flow, and 300 g of "7-MAC" and 100 g of dimethylaniline were added in batches. Stir overnight at -20°C. The solvent was evaporated to dryness under reduced pressure, 1000 ml of water and 2000 ml of ethyl acetate were added to the residue, the organic phase was separated, washed with water, and the solvent was evaporated to dryness under reduced pressure to obta...

Embodiment 2

[0037] The refining of embodiment 2 formula I intermediate

[0038] Add 100 g of the crude intermediate of formula I prepared according to Example 1 to 800 ml of isopropanol, stir vigorously at 20-25° C. for 2 hours, and then keep it overnight. After filtration, the filter cake was vacuum-dried at room temperature to obtain 82 grams of light yellow powdery solid, HPLC purity: 95.6%.

Embodiment 3

[0039] The refining of embodiment 3 formula I intermediate

[0040] Add 50 g of the crude intermediate of formula I prepared according to Example 1 to 200 ml of isopropanol, stir vigorously at 20-25° C. for 2 hours, and then keep it overnight. After filtration, the filter cake was vacuum-dried at room temperature to obtain 45 g of light yellow powdery solid, HPLC purity: 93.0%.

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Abstract

The invention relates to a refining method to prepare cefbuperazone intermediate compound with formulaI, aiming at providing a method to replace current column chromatography method to prepare cefbuperazone intermediate compound for economic and large-scale production. Cefbuperazone intermediate compound with formulaI is refined in isopropanol and highly pure product is obtained after separation process. Sodium salt of cefbuperazone is an antibiotic for cephamycins.

Description

technical field [0001] The present invention relates to the preparation method of cefbuperazone intermediate. The method is suitable for the industrial large-scale preparation of the cephamycin antibiotic-cephbuperazone sodium. Background technique [0002] Cefbuprazone Sodium (Cefbuprazone Sodium) is a cephamycin antibiotic developed by Japan Toyama Chemical Company and listed in 1985. Cefbuperazone Sodium has the chemical structure shown in the following formula: [0003] [0004] The literature describing the preparation method of cefbuperazone sodium is mainly found in the patent JP55141491 (equivalent patent: GB2048241) of the Japanese Toyama Chemical Company of the original researcher. In this patent, the synthetic method of cefbuperazone mainly contains 2 types: [0005] 1. Carry out the 7-position docking first, then introduce the methoxyl group, then remove the 4-position protecting group and other steps to obtain cefbuperazone: [0006] [0007] In this t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D501/36
Inventor 董少华徐林刘实沈小俊
Owner NANJING HAILING TRADITIONAL CHINESE MEDICINE RES CO LTD
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