Method for refining cefpiramide acid

A technology of cefpiramide and a purification method, applied in the field of medicine, can solve the problems of unfavorable industrialized production, low weight yield and high production cost, and achieve the effects of effective recycling, high purity and low production cost

Active Publication Date: 2019-03-08
NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In the literature "the synthesis of cefpiramide" (author Chen Lin etc.), about the preparation of cefpiramide finished product, the weight yield after refining is relatively low, and the total yield only has 71.2%, and the production cost is high, which is unfavorable for suitability for suitability for industrialized production

Method used

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  • Method for refining cefpiramide acid
  • Method for refining cefpiramide acid
  • Method for refining cefpiramide acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] A method for refining cefpiramin, the specific method for refining is as follows:

[0034] First put 20g of cefpiramic acid crude raw material into the mixed solution of 30ml of methanol and 30ml of dichloromethane, then add 3.2ml of triethylamine, control the temperature at 15°C, stir to dissolve, then add 0.2g of activated carbon for decolorization for 0.5h, filter Collect the filtrate; control the temperature of the filtrate at 10°C, add 100ml of dichloromethane, separate out cefpiramide salt solid crystals, filter; put the solid crystals into a mixed solution of 100ml water and 100ml isopropanol, control the temperature at 10°C, and add 20% Adjust the pH value to 2.0 with hydrochloric acid, add 20mg of seed crystals, precipitate cefpiramic acid, grow the crystals for 0.5h, filter to obtain cefpiramic acid solid crystals and mother liquor; wash cefpiramic acid solid crystals with 100ml of isopropanol, and dry at 40°C , the pressure is -0.09~-0.07MPa during drying, an...

Embodiment 2

[0037] The production process steps in this embodiment are the same as in Example 1. The difference is that the mother liquor is applied mechanically in this embodiment, specifically for dissolving the cefpiramide salt solid crystallization with the mother liquor preserved in Example 1, and all the other process parameters are the same as those in Example 1. Example 1 is the same.

Embodiment 3～6

[0039] Embodiments 3-6 are identical to the production process steps in Embodiment 1, and the difference is the selection of process parameters, as shown in Table 1, wherein:

[0040] "Amount of solvent 1" is the number of milliliters of solvent 1 added to the number of times the weight of the raw material in grams;

[0041] "Molar ratio of transamination agent" refers to the molar ratio of transamination agent to cefpiramin crude product;

[0042] "Depigmentation agent dosage" is the percentage by weight that depigmentation agent weight accounts for cefpiramide crude product;

[0043] "Dissolving agent dosage" is how many times the number of milliliters of dissolving agent is the weight of cefpiramin crude product in grams;

[0044] "Amount of solvent 2" is how many milliliters of solvent 2 is added to the number of grams of solid crystal weight obtained in step C;

[0045] "Amount of seed crystals" is the percentage by weight of the seed crystal weight in the cefpiramin cr...

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Abstract

The invention discloses a method for refining cefpiramide acid, and belongs to the technical field of medicines. The method comprises the following steps: A, putting crude cefpiramide acid into a solvent 1, adding a transaminating agent, stirring and dissolving the mixture to clarification, so as to obtain a cefpiramide salt solution; B, adding a decolorizing agent into the cefpiramide salt solution, filtering and collecting filtrate; C, controlling the filtrate temperature to be 10-20 DEG C, adding a dissolution agent, filtering and collecting a solid crystal; D, putting the solid crystal into a solvent 2, controlling the temperature to be 10-15 DEG C, adding an acidic reagent to adjust the pH value to 2.0-3.0, adding a seed crystal, crystallizing, filtering and collecting the solid crystal of cefpiramide acid and mother liquor; and E, washing the solid crystal of cefpiramide acid and drying to obtain refined cefpiramide acid. The cefpiramide acid prepared with the method is high in purity, few in impurities and low in color grade; and the refining method provided by the invention has the advantages of being simple in process, environmentally friendly, and suitable for large-scaleindustrial production, saving energy, and the like.

Description

technical field [0001] The invention relates to cephalosporins, in particular to a refining method, which belongs to the technical field of medicine. Background technique [0002] Cefpiramide is a third-generation cephalosporin, jointly developed by Sumitomo Pharmaceutical Co., Ltd. and Yamanouchi Pharmaceutical Co., Ltd., and first listed in Japan in 1985. This product has a broad antibacterial spectrum and good antibacterial activity against Gram-positive cocci. At the same time, it has high-efficiency antibacterial activity against Gram-negative bacilli, has a perfect balanced antibacterial spectrum, has good pharmacokinetic characteristics, and has good stability against β-lactamase. [0003] The chemical name of cefpiramide is (6R,7R)-7-[(R)-2-(4-hydroxy-6-methyl-3-pyridine)carboxamido-2-(4-hydroxyphenyl) -Acetamido]-3-(1-methyl-1H-tetrazole-5-thiomethyl)-8-oxo-5-thia-1-azabicyclo[4.2.0]octane-2 -ene-2-carboxylic acid. The structural formula is as follows: [0004] ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/36C07D501/04C07D501/12
CPCC07D501/04C07D501/12C07D501/36
Inventor 田洪年贾全石春利李庆伟刘树斌任峰张素霞宋玮
Owner NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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