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Purification method of cefcapene pivoxil precursor acid BCN

A technology of cefcapene pivoxil and purification method, which is applied in the field of purification of cefcapene pivoxil precursor acid BCN, can solve the problems of many by-products, low purity of BCN, inability to guarantee the quality of cefcapene pivoxil hydrochloride products, etc. Quality, Purity and Yield Improvement Effects

Active Publication Date: 2020-04-21
湖北凌晟药业股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Aiming at the many by-products in the synthesis process of the existing cefcapene pivoxil precursor acid BCN, the quality problem of the cefcapene pivoxil hydrochloride product that the purity of BCN is obtained is lower and cannot be guaranteed, the invention provides a kind of cefcapene pivoxil precursor Purification method of acid BCN

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] . a purification method of cefcapene pivoxil precursor acid BCN, comprising the following steps:

[0024] a, the BCN crude product is added to dissolve in the methanol whose weight is 5 times of the BCN crude product weight, adjust the pH to be 3 with sulfuric acid, then add the chloroform and the water whose weight is 3 times of the BCN crude product weight and the same weight as the BCN crude product weight, carry out Extraction, collecting the organic layer;

[0025] b. Add water with the same volume as the organic layer solution to the collected organic layer solution, let it stand for stratification, and collect the organic layer solution. After the above washing process is repeated twice, add anhydrous water having the same weight as the BCN crude product to the organic layer solution. Magnesium sulfate, suction filtration obtains organic layer solution;

[0026] c. Add diisopropylamine with the same molar weight as BCN to the dehydrated organic layer solution dr...

Embodiment 2

[0029] A purification method of cefcapene pivoxil precursor acid BCN, comprising the following steps:

[0030] a, the BCN crude product is added to dissolve in the methanol that the weight is 8 times of the BCN crude product weight, adjust the pH with sulfuric acid to be 3.3, add the chloroform that the weight is 4 times of the BCN crude product weight and the water that the weight is 1.5 times of the BCN crude product weight, Carry out extraction, collect organic layer;

[0031] b. Add water 1.5 times the volume of the organic layer solution to the collected organic layer solution, let stand for stratification, and collect the organic layer solution. After the above washing process is repeated 3 times, add 1.5 times the weight of the BCN crude product to the organic layer solution. Calcium, obtained by suction filtration to obtain the organic layer solution;

[0032] c. Add 1.2 times the molar amount of BCN diisopropylamine dropwise to the dehydration-treated organic layer s...

Embodiment 3

[0035] A purification method of cefcapene pivoxil precursor acid BCN, comprising the following steps:

[0036] a, the BCN crude product is added to the methanol whose weight is 10 times of the BCN crude product weight and dissolved, and the pH is adjusted to 3.5 with hydrochloric acid. Carry out extraction, collect organic layer;

[0037] B, add the water of 2 times of the volume of organic layer solution in the organic layer solution of collection, leave standstill stratification, collect organic layer solution, after the above-mentioned washing process repeats 2 times, add BCN crude product weight 2 times of non-alcohol in the organic layer solution Sodium sulfate water was obtained by suction filtration to obtain the organic layer solution;

[0038] c. Add 1.5 times the molar amount of BCN diisopropylamine dropwise to the dehydration-treated organic layer solution, and let the crystal grow for 90 minutes at 10°C, filter the crystal, wash it with water, and dry it to consta...

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Abstract

The invention relates to the technical field of medicine purification, and particularly discloses a purification method of cefcapene pivoxil precursor acid BCN. The purification method comprises the following steps: a, adding crude BCN into methanol, dissolving, adjusting the pH value to 3.0-3.5, adding trichloromethane, adding water for extraction, and collecting an organic layer; b, carrying outwater washing and dehydration treatment on the collected organic layer solution; and c, adding diisopropylamine into the dehydrated organic layer solution according to a molar ratio of the addition amount of diisopropylamine to the addition amount of the crude BCN product is (1.0-1.5):1, and standing for crystal growth at the temperature of 0-10 DEG C to obtain purified BCN crystals. The purification method makes the purity of the BCN crystal reach 99.5% or above.

Description

technical field [0001] The invention relates to the technical field of medicine purification, in particular to a method for purifying cefcapene axetil precursor acid BCN. Background technique [0002] Cefcapene pivoxil hydrochloride is the fourth generation of oral cephalosporin antibiotics, cefcapene pivoxil hydrochloride precursor (BCN) is the key substance of synthetic cefcapene pixil hydrochloride, BCN is composed of the core D-7-ACA and side chain BAPA Prepared by mixed anhydride preparation reaction and subsequent treatment process, BCN can also be modified to obtain a variety of cefcapene hydrochloride analogues. The existing BCN synthesis methods generally have the disadvantages of low purity and long process routes. As the prior art discloses the synthesis of thiazole acetic acid (BAPA) through reactions such as condensation of ethyl 4-chloroacetoacetate, cyclization, and introduction of protecting groups, and then amidation reaction with the mother nucleus D-7-ACA ...

Claims

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Application Information

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IPC IPC(8): C07D505/02C07D505/18
CPCC07D505/02C07D505/18
Inventor 何健金联明王西龙门万辉邹菁
Owner 湖北凌晟药业股份有限公司
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