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Crystallization method for reducing alpha-aminoadipic acid

A technology of aminoadipic acid and amino group is applied in the field of reducing the crystallization of α-aminoadipic acid, and can solve the problems such as prolonging the production cycle and reducing the total yield of 3-carboxylic acid.

Inactive Publication Date: 2019-08-23
GUANGZHOU HC PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But this method not only prolongs the production cycle, but also reduces the total yield of 3-acetoxymethyl-5-thio-7-amino-8-oxo-1-azabicyclooct-2-ene-2 ​​carboxylic acid

Method used

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  • Crystallization method for reducing alpha-aminoadipic acid
  • Crystallization method for reducing alpha-aminoadipic acid
  • Crystallization method for reducing alpha-aminoadipic acid

Examples

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Embodiment 1

[0032] Example 1. A crystallization method for removing α-aminoadipic acid from 3-acetoxymethyl-5-thio-7-amino-8-oxo-1-azabicyclooct-2-ene-2 ​​carboxylic acid method

[0033] The crystallization method for removing α-aminoadipic acid in 3-acetoxymethyl-5-sulfur-7-amino-8-oxo-1-azabicyclooct-2-ene-2 ​​carboxylic acid includes the following step:

[0034] S1, ultrafiltration to 1000mL (10g / L) 3-acetoxymethyl-5-sulfur-7-amino-8-oxo-1-azabicyclooct-2-ene-2carboxylic acid obtained by one-step enzymatic method α-aminoadipic acid contained in 3-acetoxymethyl-5-thio-7-amino-8-oxo-1-azabicyclooct-2-ene-2carboxylic acid ultrafiltrate The molar concentration of 3-acetoxymethyl-5-sulfur-7-amino-8-oxo-1-azabicyclooct-2-ene-2 ​​carboxylic acid is 0.1 times the molar concentration of 3-acetoxymethyl-5-sulfur-7-amino-8-oxo-1-azabicyclooct-2-ene-2carboxylic acid. Add 2mL of auxiliary solvent ethanol, Adjust the temperature of the system to 30°C to obtain an ultrafiltration mixed solution; ...

Embodiment 2

[0037] Example 2, a crystallization for removing α-aminoadipic acid from 3-acetoxymethyl-5-thio-7-amino-8-oxo-1-azabicyclooct-2-ene-2 ​​carboxylic acid method

[0038] The crystallization method for removing α-aminoadipic acid in 3-acetoxymethyl-5-sulfur-7-amino-8-oxo-1-azabicyclooct-2-ene-2 ​​carboxylic acid includes the following step:

[0039] S1, ultrafiltration to 1000mL (10g / L) 3-acetoxymethyl-5-sulfur-7-amino-8-oxo-1-azabicyclooct-2-ene-2carboxylic acid obtained by one-step enzymatic method α-aminoadipic acid contained in 3-acetoxymethyl-5-thio-7-amino-8-oxo-1-azabicyclooct-2-ene-2carboxylic acid ultrafiltrate The molar concentration of 3-acetoxymethyl-5-sulfur-7-amino-8-oxo-1-azabicyclooct-2-ene-2 ​​carboxylic acid is 2 times that of 3-acetoxymethyl-5-sulfur-7-amino-8-oxo-1-azabicyclooct-2-ene-2 ​​carboxylic acid, add 1mL of auxiliary solvent methanol, Adjust the temperature of the system to 25°C to obtain an ultrafiltration mixed solution;

[0040] S2. Add dropwis...

Embodiment 3

[0042] Example 3, a crystallization for removing α-aminoadipic acid from 3-acetoxymethyl-5-thio-7-amino-8-oxo-1-azabicyclooct-2-ene-2carboxylic acid method

[0043] The crystallization method for removing α-aminoadipic acid in 3-acetoxymethyl-5-sulfur-7-amino-8-oxo-1-azabicyclooct-2-ene-2 ​​carboxylic acid includes the following step:

[0044] S1, ultrafiltration to 1000mL (10g / L) 3-acetoxymethyl-5-sulfur-7-amino-8-oxo-1-azabicyclooct-2-ene-2carboxylic acid obtained by one-step enzymatic method α-aminoadipic acid contained in 3-acetoxymethyl-5-thio-7-amino-8-oxo-1-azabicyclooct-2-ene-2carboxylic acid ultrafiltrate The molar concentration of 3-acetoxymethyl-5-thio-7-amino-8-oxo-1-azabicyclooct-2-ene-2 ​​carboxylic acid is 0.8 times that of the molar concentration of 3-acetoxymethyl-5-thio-7-amino-8-oxo-1-azabicyclooct-2-ene-2 ​​carboxylic acid. Add 3 mL of auxiliary solvent acetone, Adjust the system temperature to 20°C to obtain an ultrafiltration mixed solution;

[0045] ...

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Abstract

The invention relates to a crystallization method of 3-acetyloxymethyl-5-thio-7-amino-8-oxo-1-azabicyclooctyl-2-ene-2-carboxylic acid, and in particular relates to a crystallization method for removing alpha-aminoadipic acid in the 3-acetyloxymethyl-5-thio-7-amino-8-oxo-1-azabicyclooctyl-2-ene-2-carboxylic acid. The method comprises the following steps: adding carboxylic acid ultrafiltrate into areactor, adding an appropriate amount of assisted solvents, regulating the pH value to a certain range value with an acid of a proper concentration, crystallizing, growing the grain and filtering, washing with acid water, filtering and drying, thereby obtaining the product. According to the preparation method disclosed by the invention, the residue of the alpha-aminoadipic acid in a target compound is effectively reduced, so that a characteristic peak of the alpha-aminoadipic acid disappears when the content of impurities is reduced to be detected by IR.

Description

technical field [0001] The present invention relates to the crystallization method of 3-acetoxymethyl-5-thio-7-amino-8-oxo-1-azabicyclooct-2-ene-2 ​​carboxylic acid, in particular to the removal of 3-acetoxymethyl Method for the crystallization of α-aminoadipic acid in yl-5-thio-7-amino-8-oxo-1-azabicyclooct-2-ene-2carboxylic acid. Background technique [0002] 3-Acetoxymethyl-5-thio-7-amino-8-oxo-1-azabicyclooct-2-ene-2carboxylic acid, the chemical name is 7-amino-3-((acetyloxy)methanol base)-8-oxo-5-thia-1-azabicyclo(4,2,0)-2-ene-2-carboxylic acid, the molecular formula is C 10 h 12 N 2 o 5 S 2 , and its structural formula is shown in Structure 1: [0003] [0004] 3-Acetoxymethyl-5-thio-7-amino-8-oxo-1-azabicyclooct-2-ene-2carboxylic acid is an important mother nucleus of cephalosporins, and its downstream products include: cefotaxime , Ceftriaxone, Cefazolin, Cefuroxime, Cefoperazone, etc. 3-Acetoxymethyl-5-thio-7-amino-8-oxo-1-azabicyclooct-2-ene-2carboxylic ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/12C07D501/18
CPCC07B2200/13C07D501/12C07D501/18
Inventor 冯彩云林立东
Owner GUANGZHOU HC PHARM CO LTD
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