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Preparation method of penicillin G sulfoxide

A technology of penicillin and medium penicillin, applied in the direction of organic chemistry, can solve the problems of complex and cumbersome production process, high power operation cost, large waste water discharge, etc., and achieve the effect of short process cycle, low cost and good purity

Active Publication Date: 2013-03-13
NORTH CHINA PHARMA COMPANY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the traditional production process, penicillin G sulfoxide is generally obtained by oxidation of penicillin G industrial salt as raw material: penicillin G salt is oxidized → crystallized → filtered → washed → dried to obtain penicillin G sulfoxide, and penicillin G salt is obtained by After filtration→extraction→extraction→crystallization, the entire production process from penicillin fermentation broth to penicillin G sulfoxide is complex and cumbersome, and a large amount of solvent is used for extraction in this process, which leads to high power operation costs and waste water discharge. Large and expensive to produce

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 1000ml penicillin G fermentation broth (concentration: 90000μ / g) into a 2000ml three-neck flask, and cool down to 0~5°C in an ice-salt bath. Under rapid stirring, add dropwise peracetic acid with a concentration of 30% by mass to volume until the oxidation end point and then terminate the oxidation (use potassium iodide starch test paper to detect the oxidation end point) to obtain solution I. Solution I was filtered through a 100nm ceramic membrane to filter out solid impurities, washed with an appropriate amount of water, and filtered. The filtrate was concentrated with a nanofiltration membrane with a molecular weight cut off of FW=500. The concentrate was adjusted to PH=1-1.5 with sulfuric acid, and filtered at 0-20°C to obtain the crude penicillin G sulfoxide (wet product). Put the penicillin G sulfoxide crude product (wet product) into 60% methanol solution, and recrystallize at 40-48°C. Cool down to 0-10°C and filter. Wash with methanol at 0°C and drain. ...

Embodiment 2

[0024] Add 1000ml penicillin G fermentation broth (concentration: 95000μ / g) into a 2000ml three-neck flask, and cool down to 0~5°C in an ice-salt bath. Under rapid stirring, add dropwise peracetic acid with a mass volume ratio concentration of 33% to the oxidation end point and then terminate the oxidation (use potassium iodide starch test paper to detect the oxidation end point) to obtain solution I. Solution I was filtered through a 50nm ceramic membrane to filter out solid impurities, washed with an appropriate amount of water, and filtered. The filtrate was concentrated with a nanofiltration membrane with a molecular weight cut off of FW=200. The concentrate was adjusted to PH=1-1.5 with sulfuric acid, and filtered at 0-20°C to obtain the crude penicillin G sulfoxide (wet product). Put the penicillin G sulfoxide crude product (wet product) into 80% methanol aqueous solution, and recrystallize at 40-48°C. Cool down to 0-10°C and filter. Wash with methanol at 0°C and drai...

Embodiment 3

[0026] Add 1000ml penicillin G fermentation broth (concentration: 60000μ / g) into a 2000ml three-neck flask, and cool down to 0-8°C in an ice-salt bath. Under rapid stirring, add dropwise peracetic acid with a mass volume ratio concentration of 28% to the oxidation end point and then terminate the oxidation (use potassium iodide starch test paper to detect the oxidation end point) to obtain solution I. Solution I was filtered through a 200μm ceramic membrane to filter out solid impurities, washed with an appropriate amount of water, and filtered. The filtrate was concentrated with a nanofiltration membrane with a molecular weight cut-off FW=800. The concentrate was adjusted to PH=1-1.5 with sulfuric acid, and filtered at 0-20°C to obtain the crude penicillin G sulfoxide (wet product). Put the penicillin G sulfoxide crude product (wet product) into 9% methanol aqueous solution, and recrystallize at 35-40°C. Cool down to 0-10°C and filter. Wash with methanol at 0°C and drain. ...

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PUM

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Abstract

The invention discloses a novel method for preparing penicillin G sulfoxide, which comprises the following steps: a, selecting a 60000-120000 mu / g penicillin G fermentation solution, and dropwisely adding peroxyacetic acid to obtain a solution I; b, filtering the solution I to obtain a filtrate, and concentrating the filtrate through a nanofiltration membrane of which the molecular weight cut-off is 200-800Da, thus obtaining a concentrated solution; c, regulating the pH value of the concentrated solution with sulfuric acid, and filtering to obtain a penicillin G sulfoxide crude product; and d, dissolving the penicillin G sulfoxide crude product in a methanol water solution, recrystallizing, then cooling to 0-10 DEG C, filtering, washing the obtained crystals with methanol, swabbing off, and performing microwave drying on the obtained product to obtain the penicillin G sulfoxide. According to the invention, the method is simple, the process period is short, and extraction treatment can be performed without using a large amount of organic solvent. Thus, the method disclosed by the invention is low in cost and environment-friendly.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering crystallization, and in particular relates to a preparation method of penicillin G sulfoxide. Background technique [0002] Penicillin sulfoxide is a very important intermediate in the conversion process of penicillin to cephalosporin. In the traditional production process, penicillin G sulfoxide is generally obtained by oxidation of penicillin G industrial salt: penicillin G salt is oxidized → crystallized → filtered → washed → dried to obtain penicillin G sulfoxide, and penicillin G salt is obtained by After filtration→extraction→extraction→crystallization, the entire production process from penicillin fermentation broth to penicillin G sulfoxide is complicated and cumbersome, and a large amount of solvent is used for extraction in this process, which leads to high power operation costs and waste water discharge. Large and expensive to produce. Currently, a simplified method for t...

Claims

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Application Information

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IPC IPC(8): C07D499/46C07D499/04
Inventor 魏青杰段志钢刘东张锁庆米振瑞刘明儒付成明王东杨帆张苗静郑宝丽高俊艳冯立峰
Owner NORTH CHINA PHARMA COMPANY
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