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Production method of penicillin sulfoxide industrial products

A technology of penicillin sulfoxide and production method, which is applied in the field of medicine and chemical industry, can solve the problems of quality and yield reduction, difficulty in drying and separation, and achieve the effects of improved stability, easy drying and easy separation

Pending Publication Date: 2021-02-12
NORTH CHINA PHARMA COMPANY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The crystal is dihydrate, the crystal is small, difficult to separate, difficult to wash impurities, and even more difficult to dry. It can only be used for the next process, and cannot be a commodity that is easy to store and transport.
Patent CN101239984A and patent CN102964355A introduce the method of recrystallization through crystal transformation, but the operation of crystal transformation at 50-60°C is adopted, and the product is damaged by temperature, resulting in a decrease in quality and yield, dissolution, crystal transformation, and crystallization Miscible control is difficult to meet the refinement of poor quality products

Method used

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  • Production method of penicillin sulfoxide industrial products

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Effect test

Embodiment 1

[0033] Suspend 200 grams of penicillin sulfoxide dihydrate (content 70.2%) in 200 ml of methanol, under stirring at 10°C, add 360 ml of methanol and 50 ml of 20% ammonia water for 1 hour to dissolve in methanol aqueous solution, and filter the solution with diatomaceous earth , under the condition of stirring at 10°C, add 40ml of methanol and 200ml of 20% sulfuric acid in 1 hour to crystallize in aqueous methanol solution, grow crystals for 30 minutes, filter, wash with 200ml of 80% aqueous methanol, and dry at 50°C for 1 hour to obtain 147.6 grams of penicillin sulfoxide (content 91.5%, loss on drying 8.6%, light absorption 0.004, light transmission 95.8%), yield 96.2%.

Embodiment 2

[0037] Suspend 100 grams of penicillin sulfoxide methanolate (content 90.6%) in 100 ml of methanol, under stirring at 10°C, add 30 ml of methanol and 25 ml of 20% ammonia water for 1 hour to dissolve in methanol aqueous solution, and filter the solution with diatomaceous earth. Under stirring conditions at 10°C, add 20ml of methanol and 100ml of 20% sulfuric acid in 1 hour to crystallize in an aqueous methanol solution mixed with crystallization for 30 minutes, filter, wash with 100ml of 80% aqueous methanol, and dry at 50°C for 1 hour to obtain 95.8 grams of penicillin sulfoxide (content 91.6%, loss on drying 8.6%, light absorption 0.002, light transmission 98.2%), yield 96.9%.

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Abstract

The invention discloses a production method of penicillin sulfoxide industrial products, which belongs to the field of pharmaceutical chemicals. The method adopts the scheme that penicillin sulfoxideis suspended in a methanol or methanol aqueous solution, alkaline solution is added under the condition of stirring to dissolve penicillin sulfoxide, filtrate is obtained by filtering, an acid solution is added into the filtrate for crystallization, filtering and washing are carried out, and drying is performed to obtain a penicillin sulfoxide industrial product. The production method disclosed bythe invention is universally suitable for refining penicillin sulfoxide with various qualities prepared by various methods, the penicillin sulfoxide obtained by crystal transformation at normal temperature or low temperature is good in quality and high in yield, impurities are easy to separate and wash, the product is easy to dry, the stability is greatly improved, and the penicillin sulfoxide becomes a circulating commodity; in the obtained product, the penicillin sulfoxide content is more than or equal to 91.0 percent, the drying weight loss is less than or equal to 9.0 percent, the content(pure) is more than or equal to 99.9 percent, the light absorption (425nm) is less than or equal to 0.01, and the light transmission (425nm) is more than or equal to 90 percent.

Description

technical field [0001] The invention relates to a production method of penicillin sulfoxide, in particular to a production method of an industrial product of penicillin sulfoxide, which belongs to the field of medicine and chemical industry. Background technique [0002] Penicillin Sulfoxide (Penicillin Sulfoxide), the chemical name is (2S,5R,6R)-3,3-dimethyl-6-(2-phenylacetamido)-7-oxo-4-thia-1-aza Heterobicyclo[3.2.0]heptane-2-carboxylic acid-4-oxide, molecular formula C 16 h 18 o 5 N 2 S, molecular weight is 350.2, its chemical structure formula is as follows: [0003] [0004] Penicillin sulfoxide is an important raw material for the production of cephalosporin drugs, and is a key intermediate in the step of ring expansion from the five-membered ring structure of penicillin to the six-membered ring structure of cephalosporins. Various cephalosporins can be synthesized by penicillin sulfoxide through ring expansion and rearrangement reactions Acids such as 7-ADCA ...

Claims

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Application Information

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IPC IPC(8): C07D499/46C07D499/18
CPCC07D499/18C07D499/46
Inventor 闫峰段志钢张伟赵伟马利科刘伟边永亮杨忠辉谷中芝
Owner NORTH CHINA PHARMA COMPANY
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