Technology for hydrolyzing D-(-)-p-hydroxyphenylglycine-p-toluenesulfonate

A technology of p-hydroxyphenylglycine and toluene sulfonate is applied in the production field of pharmaceutical chemical intermediates and can solve the problems of low yield, poor quality and high cost of L-p-hydroxyphenylglycine

Inactive Publication Date: 2010-06-30
HENAN NEWLAND PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The L-p-hydroxyphenylglycine obtained by hydrolysis before the present invention has low yield (yield no more than 38%) and poor quality (content ≤ 98%, light absorption ≥ 0.10), so the cost is higher, the quality is poor, and there is no market competitiveness

Method used

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  • Technology for hydrolyzing D-(-)-p-hydroxyphenylglycine-p-toluenesulfonate
  • Technology for hydrolyzing D-(-)-p-hydroxyphenylglycine-p-toluenesulfonate

Examples

Experimental program
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Effect test

Embodiment Construction

[0015] 1. First add 2500 kg of pure water into the 5000L reactor, start stirring and put in 1000 kg of purified D salt, and open the steam valve to raise the temperature.

[0016] 2. After heating up and dissolving, add 10 kg of activated carbon for decolorization, keep warm at 85-90°C for 30 minutes, and then filter while it is hot.

[0017] 3. Add 5 kg of EDTA catalyst to the filtered mother liquor, neutralize it with ammonia water, and adjust the pH between 4.2-4.4.

[0018] 4. Cool down to 30°C and keep warm for 2 hours, then centrifuge.

[0019] 450-460 kg of pure L-p-hydroxyphenylglycine can be obtained, and the quality is as follows:

[0020] Content≥99.5%

[0021] Absorption≤0.050

[0022] Optical rotation: -156°~-161°

[0023] Single impurity≤1ppm

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Abstract

The invention discloses a technology for hydrolyzing D-(-)-p-hydroxyphenylglycine-p-toluenesulfonate, which belongs to the field of the production of pharmaceutical and chemical intermediates and relates to a technology for hydrolyzing a compound having the following structure. The traditional D-p-hydroxyphenylglycine obtained by hydrolysis has low yield (not more than 38 percent) and low quality (the content of not more than 98 percent and the light absorption of not smaller than 0.10), therefore, the cost is higher, and the quality is low without market competitive force. The invention overcomes the defects, improves the yield (not smaller than 45 percent) and the production quality (the content of not smaller than 99.5 percent, the light absorption of not more than 0.050, the optical rotation of minus156-minus 161 degrees and single impurities of not more than 1ppm), has easy acquisition of needed raw materials, lower production cost and simple and easily-applied operation and meets the requirement of enterprise development.

Description

technical field [0001] The invention belongs to the field of production of pharmaceutical and chemical intermediates, and relates to the hydrolysis technology for compound products with the following structure: [0002] [0003] The chemical name is D-(-)-p-hydroxyphenylglycine p-toluenesulfonate, which can be hydrolyzed to obtain L-p-hydroxyphenylglycine, which is the side chain of semi-synthesized amoxicillin and cefadroxil. Background technique [0004] The L-p-hydroxyphenylglycine obtained by hydrolysis before the present invention has low yield (yield no more than 38%) and poor quality (content ≤ 98%, light absorption ≥ 0.10), which has high cost, poor quality and no market competitiveness. The present invention overcomes the above disadvantages, improves the yield (yield ≥ 45%), and improves product quality (content ≥ 99.5%; light absorption ≤ 0.050; optical rotation: -156°~-161°; single impurity ≤ 1ppm). The required raw materials are easy to obtain, and the produ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C229/22C07C227/00C07C227/30
Inventor 谢建中
Owner HENAN NEWLAND PHARMA
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