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A kind of manufacture method of d-l-p-hydroxyphenylglycine

A technology of p-hydroxyphenylglycine and a manufacturing method is applied in chemical instruments and methods, preparation of organic compounds, preparation of cyanide reaction, etc., can solve problems such as heating and long reaction time, and achieve the effect of convenient operation

Inactive Publication Date: 2011-12-21
HENAN NEWLAND PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It also has the disadvantages of heating and long reaction time

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] Technical scheme of the present invention is realized like this:

[0011] (1), by weight 1000 grams of water, 50 grams of urea, 50 grams of potassium chlorate mixed configuration solution is standby as reaction solution;

[0012] (2) Add 265 grams of phenol: 477 grams of sulfamic acid: 212 grams of glyoxylic acid in the above-mentioned 1060 grams of reaction liquid according to the weight ratio, react at 20° C. for 2 hours and filter to obtain D-L-p-hydroxyphenylglycine crystals. The single-pass yield can reach 66.9%, and the yield after recovery of the mother liquor can reach 81.2%.

Embodiment 2

[0014] Technical scheme of the present invention is realized like this:

[0015] (1), by weight 1000 grams of water, 50 grams of urea, 50 grams of potassium chlorate mixed configuration solution is standby as reaction solution;

[0016] (2) Add 330 grams of phenol: 550 grams of sulfamic acid: 275 grams of glyoxylic acid in the above 1100 grams of reaction liquid according to the weight ratio, react at 30° C. for 1 hour and filter to obtain D-L-p-hydroxyphenylglycine crystals. The single-pass yield can reach 64.3%, and the yield after recovery of the mother liquor can reach 81.0%.

Embodiment 3

[0018] Technical scheme of the present invention is realized like this:

[0019] (1), by weight 1000 grams of water, 50 grams of urea, 30 grams of potassium chlorate mixed configuration solution is standby as reaction solution;

[0020] (2) Add 270 grams of phenol: 550 grams of sulfamic acid: 270 grams of glyoxylic acid in the above-mentioned 1080 grams of reaction liquid according to the weight ratio, react at 25° C. for 1.5 hours and filter to obtain D-L-p-hydroxyphenylglycine crystals.

[0021] The single-pass yield can reach 65.9%, and the yield after recovery of the mother liquor can reach 81.1%.

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PUM

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Abstract

The invention relates to the fields of chemical industry and pharmaceutical production, in particular to a method for producing D-L-p-hydroxyphenylglycine. The technical scheme of the present invention is achieved like this: (1) by weight water: urea: potassium chlorate=100: 3-5: 3-5 configuration solution is standby as reaction solution; (2) drop into in above-mentioned reaction solution according to weight ratio Reaction solution: phenol: sulfamic acid: glyoxylic acid = 20:5-6:9-10:4-5, react at 20-30°C for 1-2 hours and filter to obtain D-L-p-hydroxyphenylglycine crystals. Such a method for producing D-L-p-hydroxyphenylglycine is easy to operate and does not require the effect of heating.

Description

technical field [0001] The invention relates to the fields of chemical industry and pharmaceutical production, in particular to a method for producing D-L-p-hydroxyphenylglycine. Background technique [0002] D-L-p-Hydroxyphenylglycine is mainly used in the production of amoxicillin, amoxicillin clavulanate, etc. The current synthesis method mainly has the molar ratio of phenol: sulfamic acid: glyoxylic acid = 1: 1.2: 1, using water as a solvent and concentrated sulfuric acid as a catalyst. Control the temperature at 50-60° C. and react for 5-6 hours. It also has the disadvantages of heating and long reaction time. Contents of the invention [0003] Purpose of the present invention is exactly for above-mentioned shortcoming, a kind of temperature is not required, the manufacture method of D-L-p-hydroxyphenylglycine with short reaction time is provided. [0004] Technical scheme of the present invention is realized like this: [0005] (1), by weight water: urea: potassi...

Claims

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Application Information

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IPC IPC(8): C07C229/36C07C227/10
Inventor 谢建中张芦苇刘万民
Owner HENAN NEWLAND PHARMA
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