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Subsequent treatment method for enzymatic synthesis of D-p-hydroxyl phenyl glycine

A technology of p-hydroxyphenylglycine and enzymatic synthesis, which is applied in the fields of organic chemistry methods, chemical instruments and methods, and preparation of organic compounds, etc., can solve the problems such as difficulty in removing impurities by filter membrane, affecting product quality, and unqualified alkali absorbance. , to achieve the effect of reducing the difficulty of environmental protection treatment, realizing rational utilization, and reducing production costs

Active Publication Date: 2021-08-06
INNER MONGOLIA CHANGSHENG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is difficult to remove impurities from the filter membrane thoroughly, and the remaining impurities will denature and develop color under strong alkaline conditions, resulting in unqualified alkali absorbance and affecting product quality.

Method used

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  • Subsequent treatment method for enzymatic synthesis of D-p-hydroxyl phenyl glycine
  • Subsequent treatment method for enzymatic synthesis of D-p-hydroxyl phenyl glycine
  • Subsequent treatment method for enzymatic synthesis of D-p-hydroxyl phenyl glycine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0068] Such as figure 1 As shown, take the first batch of enzymatically synthesized D-hydroxyphenylglycine reaction feed solution 2m 3 processing, including the following steps:

[0069] (1) oxidation

[0070] Use concentrated ammonia water to adjust the pH of the feed solution obtained by the enzymatic synthesis of D-hydroxyphenylglycine to 10.1, and add 10kg of hydrogen peroxide (after testing, this dose can ensure the maximum oxidation effect of the oxidized feed liquid) under slow stirring conditions, and oxidize for 2 hours , to obtain the oxidized feed solution.

[0071] (2) dilution

[0072] The oxidizing feed liquid is transferred to the dilution tank and diluted with water to about 9.0m 3 , to obtain a dilution of D-p-hydroxyphenylglycine.

[0073] (3) Decolorization

[0074] Use 30% hydrochloric acid to adjust the pH of the D-p-hydroxyphenylglycine dilution to 5.0, add 30 kg of activated carbon and slowly stir (70 r / min) for adsorption for 30 minutes, and filte...

Embodiment 2

[0087] Take the second batch of enzymatically synthesized D-hydroxyphenylglycine reaction feed solution 2m 3 processing, including the following steps:

[0088] (1) oxidation

[0089] Use concentrated ammonia water to adjust the pH of the feed solution obtained by enzymatically synthesizing D-p-hydroxyphenylglycine to 10.1, add 10 kg of hydrogen peroxide under slow stirring conditions, and oxidize for 2 hours to obtain an oxidized feed solution.

[0090] (2) dilution

[0091] The oxidized feed liquid is transferred to the dilution tank, diluted with the washing water obtained in Example 1, condensed water and the trivalent salt feed liquid, and then diluted with water to about 9.5m 3 , to obtain a dilution of D-p-hydroxyphenylglycine.

[0092] (3) Decolorization

[0093] Use 30% hydrochloric acid to adjust the pH of the D-p-hydroxyphenylglycine dilution to 5.0, add 30 kg of activated carbon and slowly stir (70 r / min) for adsorption for 30 minutes, and filter the activated ...

Embodiment 3

[0105] Take the second batch of enzymatically synthesized D-hydroxyphenylglycine reaction feed solution 2m 3 processing, including the following steps:

[0106] (1) oxidation

[0107] Use concentrated ammonia water to adjust the pH of the feed liquid obtained by enzymatically synthesizing D-p-hydroxyphenylglycine to 10.2, add 10 kg of hydrogen peroxide under slow stirring conditions, and oxidize for 2 hours to obtain an oxidized feed liquid.

[0108] (2) dilution

[0109] The oxidized feed liquid is transferred to the dilution tank, diluted with the washing water obtained in Example 2, condensed water and the trivalent salt feed liquid, and then diluted with water to about 9.5m 3 , to obtain a dilution of D-p-hydroxyphenylglycine.

[0110] (3) Decolorization

[0111] Use 30% hydrochloric acid to adjust the pH of the D-p-hydroxyphenylglycine dilution to 5.0, add 30 kg of activated carbon and slowly stir (70 r / min) for adsorption for 30 minutes, and filter the activated carb...

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Abstract

The invention discloses a subsequent treatment method for enzymatic synthesis of D-p-hydroxyl phenyl glycine, and relates to the field of chemical pharmacy, and the subsequent treatment method comprises the following steps: (1) oxidation: adjusting the pH value of a feed liquid obtained by a reaction for enzymatic synthesis of D-p-hydroxyl phenyl glycine to be alkaline, and adding hydrogen peroxide for oxidation to obtain an oxidized feed liquid; (2) dilution: adding water into the oxidized feed liquid for dilution to obtain a D-p-hydroxyl phenyl glycine diluent; (3) decoloring: adjusting the pH value of the D-p-hydroxyl phenyl glycine diluent to be acidic, adding activated carbon to adsorb and remove impurities, and filtering the activated carbon to obtain a D-p-hydroxyl phenyl glycine decolored solution; and (4) preparation of a finished product: carrying out reverse osmosis concentration on the D-p-hydroxyl phenyl glycine decolored solution to separate out D-p-hydroxyl phenyl glycine, and filtering, washing and drying to obtain the finished product D-p-hydroxyl phenyl glycine. The method is simple in process, good in impurity removal effect, excellent in finished product quality and suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of chemical industry and pharmacy, in particular to a subsequent treatment method for enzymatically synthesizing D-p-hydroxyphenylglycine. Background technique [0002] D-p-hydroxyphenylglycine (D-p-HPG, D-HPG) is an important intermediate in the manufacture of semi-synthetic penicillins and semi-synthetic cephalosporins, and can be used to synthesize broad-spectrum antibiotics amoxicillin, cefadroxil, cephalosporin Piperidone, Cefarozil, etc. [0003] At present, the methods for preparing D-p-hydroxyphenylglycine mainly include bio-enzyme catalysis and chemical synthesis. The bio-enzyme catalysis has less environmental pollution and mild reaction conditions, and has gradually become a research hotspot. [0004] The preparation of D-p-hydroxyphenylglycine by biological enzyme catalysis mainly uses p-hydroxyphenylhydantoin (DL-HPH) as the substrate, and uses D-hydantoinase (IDH) to convert it into N-carbamoy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C229/36C07C227/40
CPCC07C227/40C07B2200/07C07C229/36
Inventor 陈顺记郭建明徐德芳程炜袁晓明高建成郝海涛白雪峰沈张宁
Owner INNER MONGOLIA CHANGSHENG PHARMA