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A kind of preparation method of cephalexin raw material and capsule

A technology of cephalexin and raw materials, applied in the field of medicine, can solve the problems of affecting the yield, difficulty in enzyme separation, and low production efficiency, and achieve the effects of increasing production yield, overcoming difficulties in enzyme separation, and improving production efficiency

Active Publication Date: 2019-04-12
NORTH CHINA PHARMA COMPANY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But it still has many unsatisfactory parts, as: there is more serious enzyme separation difficulty in its enzymatic condensation reaction process of the technique of existing enzymatic synthesis cephalosporin, thus greatly affects yield, causes production efficiency to be low

Method used

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  • A kind of preparation method of cephalexin raw material and capsule
  • A kind of preparation method of cephalexin raw material and capsule
  • A kind of preparation method of cephalexin raw material and capsule

Examples

Experimental program
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Effect test

Embodiment 1

[0025] A preparation method of cephalexin raw material, comprising the following steps:

[0026] (1) Add 120ml of deionized water and 20g of 7-ADCA in the reaction flask, stir to dissolve, and dissolve L-phenylglycine methyl ester hydrochloride (18.0g in terms of L-phenylglycine methyl ester) with 50ml of deionized water. The solution was slowly added to the 7-ADCA aqueous solution within 45 minutes, then 15 g of immobilized penicillin acylase (with an activity of 23 U / g) was added, and the acylation reaction was carried out at 15 ° C. The reaction time was 3.0 hours, and ammonia water was used during the reaction to maintain The pH is at 6.2.

[0027] (2) After the reaction is terminated, adjust the viscosity of the reaction solution to 50mPa·s with deionized water, and then use the penicillin acylase separator (see figure 1 ) for initial separation, the penicillin acylase separator includes a tank 1 and a cover 2 sealed thereto, the bottom of the tank 1 is provided with a b...

Embodiment 2

[0032] A preparation method of cephalexin raw material, comprising the following steps:

[0033] (1) Add 140ml of deionized water and 20g of 7-ADCA into the reaction flask, stir to dissolve, dissolve the L-phenylglycine methyl ester sulfate (18.5g in terms of L-phenylglycine methyl ester) with 50ml of deionized water, and dissolve the solution Slowly add to 7-ADCA aqueous solution within 60min, then add 18g of immobilized penicillin acylase (activity is 23U / g), carry out acylation reaction at 18°C, the reaction time is 2.8 hours, maintain the pH with ammonia water during the reaction In 6.6.

[0034] (2) After the reaction is terminated, adjust the viscosity of the reaction solution to 100mPa·s with deionized water, and then use the penicillin acylase separator (see figure 1 ) for initial separation, the penicillin acylase separator includes a tank 1 and a cover 2 sealed thereto, the bottom of the tank 1 is provided with a bottom inlet and outlet 3 and the middle of the tank ...

Embodiment 3

[0039] A preparation method of cephalexin raw material, comprising the following steps:

[0040] (1) Add 180ml of deionized water and 20g of 7-ADCA into the reaction bottle, stir to dissolve, slowly add 21.6g of L-phenylglycine methyl ester into the 7-ADCA aqueous solution within 75min, and then add 19g of immobilized penicillin acylase (activity is 23U / g), acylation reaction is carried out at 20°C, the reaction time is 2.5 hours, and the pH is maintained at 7.0 with ammonia water during the reaction;

[0041] (2) After the reaction is terminated, adjust the viscosity of the reaction solution to 200mPa·s with deionized water, and then use the penicillin acylase separator (see figure 1 ) for initial separation, the penicillin acylase separator includes a tank 1 and a cover 2 sealed thereto, the bottom of the tank 1 is provided with a bottom inlet and outlet 3 and the middle of the tank 1 is provided with an intermediate inlet 4 , the cover 2 is provided with 6 symmetrically ar...

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Abstract

The invention discloses a preparation method of a cephalexin raw material, comprising the following steps: (1) adding an L-Phenylglycine ester derivative in a 7-ADCA aqueous solution slowly, adding immobilized penicillin acylase for reaction; (2) adjusting reaction solution viscosity, separating enzyme with a penicillin acylase separator, centrifugally filtering the cephalexin suspension, to obtain cephalexin crude powder and the filtering liquid; (3) cleaning enzyme with the filtering liquid, separating the enzyme, centrifuging the cephalexin suspension, filtering to obtain cephalexin crude powder and the filtering liquid, mixing the obtained two cephalexin crude powders; (4) repeating step (3), until the liquid flowing out is clear; and (5) mixing total cephalexin crude powders and the filtrate, adjusting pH with sulfuric acid, filtering with 0.45[mu]m filtering film to obtain a material liquid, raising the temperature of the material liquid, adjusting pH of the material liquid with ammonia water, then growing crystal, filtering the crystals, washing the crystals with water and then acetone, and drying the crystals to obtain final product of cephalexin. The cephalexin preparation method enables the cephalexin to separate easily with the enzyme.

Description

technical field [0001] The invention relates to a preparation method of a cephalexin raw material and a capsule, belonging to the field of medicine. Background technique [0002] Cephalexin (Cephalexin) is a semi-synthetic β-lactam antibiotic with broad-spectrum antibacterial effect on Gram-positive bacteria and Gram-negative bacteria. Its mechanism of action is by inhibiting the synthesis of cell walls, Swell the contents of the cells until they are ruptured and dissolved, thereby achieving a bactericidal effect. [0003] Cefalexin is a semi-synthetic oral cephalosporin antibiotic listed by Eli Lilly Company in the United States in 1970. Its chemical name is (6R, 7R)-3-methyl-7-[(R)-2-amino-2-phenylacetamido]- 8-Oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid. Cephalexin capsules were first listed on the FDA in 1971 by SHIONOGI INC (Shionogi). [0004] At present, the green synthesis process of cephalexin is enzymatic method, which has been widely described in ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C12P35/04C07D501/22A61K31/545A61K9/48A61P31/04
Inventor 段志钢王明波张军立臧飞刘倩张锁庆王新辉穆军明段素英米建伟贾玉捷杨丹郑宝丽门红乐刘雪飞吴士军李雪元王朝卿刘海席王景欣柳世萍
Owner NORTH CHINA PHARMA COMPANY
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