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Preparation method of chlorazol benzathine benzylpenicillin

A technology for chlorpyrifosin and chlorfenacil is applied in the field of preparation of chlorfenacil, can solve the problems of complex production process, many reaction steps, low product yield and the like, and achieves reduction of toxicity, reduction of occlusion, high purity effect

Active Publication Date: 2012-09-26
NORTH CHINA PHARM GRP SEMISYNTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, this product mainly adopts the process of synthesizing cloxacillin sodium from o-chlorobenzaldehyde, and then reacting with N,N'-dibenzylethylenediamine diacetate to produce cloxacillin penicillin. This process is difficult due to many reaction steps. The production process is complicated, the controllability is poor, the yield of the produced product is low, and the impurity content is high

Method used

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  • Preparation method of chlorazol benzathine benzylpenicillin
  • Preparation method of chlorazol benzathine benzylpenicillin
  • Preparation method of chlorazol benzathine benzylpenicillin

Examples

Experimental program
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Effect test

Embodiment 1

[0025] At 25°C, add 10.0g of cloxacillin sodium into 100ml of purified water, stir to dissolve, control the pH between 6.0-8.0, add 100ml of 95vl% ethanol to make solution A;

[0026] Dissolve 4.5g of N,N'-dibenzylethylenediamine diacetic acid (DBED, the same below) in 45ml of purified water, add 45ml of 95vl% ethanol to make solution B.

[0027] Pre-add 15% of the total amount of solution A to solution B, stir until the crystals appear, grow the crystals for 10 minutes, continue to feed solution A, complete the addition in 30 minutes, carry out the salt formation reaction for 4 hours, and obtain the cloxacin penicillin suspension , filtered, washed with ethyl acetate, suction filtered, and vacuum-dried at 50°C to obtain the finished product of benzathine penicillin with a yield of 90.0%, a grain size of 100 μm, a pH of 5.6, and a content of 95.1%.

Embodiment 2

[0029] At 25°C, add 15.0g of cloxacillin sodium into 30ml of purified water, stir to dissolve, control the pH between 6.0-8.0, add 10ml of 75vl% ethanol to make solution A;

[0030] Dissolve 6.4g of DBED in 40ml of purified water, add 20ml of 75% ethanol to make solution B.

[0031] Pre-add 30% of the total amount of solution A to solution B, stir until the crystals appear, grow the crystals for 10 minutes, continue to feed solution A, complete the addition in 30 minutes, carry out the salt formation reaction for 4 hours, and obtain chlorxazone penicillin suspension , filtered, washed with ethyl acetate, suction filtered, and vacuum-dried at 50°C to obtain the finished product of benzathine penicillin with a yield of 83.0%, a grain size of 100 μm, a pH of 5.6, and a content of 95.1%.

Embodiment 3

[0033] At 25°C, add 15.0g cloxacillin sodium into 150ml purified water, stir to dissolve, control the pH between 6.0-8.0, add 150ml 95% ethanol to make solution A;

[0034] Dissolve 6.4g of DBED in 12.8ml of purified water, add 6.7ml of 95% ethanol to make solution B.

[0035] Pre-add 15% of the total amount of solution B to solution A, stir until the crystals appear, grow the crystals for 30 minutes, continue to feed solution B, complete the addition in 30 minutes, carry out the salt formation reaction for 4 hours, and obtain cloxacin penicillin suspension , filtered, washed with ethyl acetate, suction filtered, and vacuum-dried at 50°C to obtain the finished product of benzathine penicillin with a yield of 90.0%, a crystal grain size of 100 μm, a pH of 5.6, and a content of 95.1%.

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Abstract

The invention relates to a preparation method of chlorazol benzathine benzylpenicillin, which comprises the following steps of: (a) measuring and taking the following materials of 1.0g of cloxacillin sodium, 2.0-10.0ml of water and 0.5-10.0ml of buffer agent according to the mass volume ratio to prepare solution A; (b) measuring and the taking the following materials of 1.0g of N, N'-DBED, 2.0-10.0ml of water and 1.0-10.0ml of buffer agent according to the mass volume ration to prepare solution B; (c) adding 15-30 percent of the total amount of the solution A into the solution B, reacting under a stirring state to generate crystal, and growing the crystal for 10-30 minutes; and flowing the rest solution A into the solution B within 30 minutes, and carrying out salt forming reaction to obtain chlorazol benzathine injectable suspension; and (d) filtering, washing, leaching, and vacuum drying at 50-80 DEG C to obtain the product. Stable degree of supersaturation is kept during the reaction, and the nucleus formation caused by outbreak of the product is effectively controlled, so that the product quality can be improved.

Description

technical field [0001] The present invention relates to the preparation method of compound, specifically the preparation method of cloxacin penicillin. Background technique [0002] Cloxacillin penicillin is a semi-synthetic broad-spectrum antibiotic. It is the dibenzylethylenediamine salt of cloxacillin sodium. Its intestinal absorption is good and rapid, and it is not disturbed by food. It has a high blood concentration and lasts for a long time , can effectively treat infections caused by Staphylococcus and Streptococcus. The chemical name of chlorbenzathine penicillin is: (2S,5R,6R)-3,3-Dimethyl-6-[5-methyl-3(2-chlorophenyl)-4-isoxazolecarboyl Amino]-7-oxo-4-thia-1-azabicyclo[3.2.0]heptane-2-carboxylic acid N,N'-dibenzylethylenediamine salt (2:1). [0003] Molecular formula: C 16 h 2 0N 2 ,(C 19 h 18 CLN 3 O 5 S) 2 Molecular weight: 1112.1 [0004] The structural formula of chlorbenzathine penicillin: [0005] [0006] At present, this product mainl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D499/76C07D499/14C07C211/27C07C209/00
Inventor 李晓宇郭秀敏安欣林张义恩郝小良金树辉骆建峰刘敏李振强焦玮李广慧
Owner NORTH CHINA PHARM GRP SEMISYNTECH CO LTD
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