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Technology for splitting DL-p-hydroxyphenylglycine-o-toluenesulfonate

A technology of hydroxyphenylglycine o-toluenesulfonate, which is applied in the field of DL-p-hydroxyphenylglycine o-toluenesulfonate separation technology, can solve the problem of no market competitiveness, low yield, and increased labor costs. Labor intensity and other issues

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

[0005] Before the present invention, the resolution rate of DL-p-hydroxyphenylglycine o-toluenesulfonate did not exceed 85%, and the unqualified materials needed to be re-cooked, which not only increased the labor intensity of workers, but also resulted in low yield and high production cost. , no market competitiveness

Method used

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  • Technology for splitting DL-p-hydroxyphenylglycine-o-toluenesulfonate
  • Technology for splitting DL-p-hydroxyphenylglycine-o-toluenesulfonate

Examples

Experimental program
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Effect test

Embodiment Construction

[0014] 1. First add 3000 kg of pure water into the 5000L reactor, start stirring, then put 1363 kg of DL-p-hydroxyphenylglycine o-toluenesulfonic acid hydrochloride, and open the steam valve to raise the temperature.

[0015] 2. Raise the temperature to 85°C and keep it at 85-90°C for 1 hour.

[0016] 3. Add 30 kg of activated carbon and decolorize, 120 kg of D-(-)-p-hydroxyphenylglycine o-toluenesulfonate, keep warm at 90-95°C for 30 minutes and filter while hot.

[0017] 4. Cool down the temperature of the filtered mother liquor to 28°C and start to measure the optical rotation. When the optical rotation is ≥+2°, discharge and centrifuge.

[0018] 5. D-(-)-p-hydroxyphenylglycine o-toluenesulfonate obtained after centrifugation: 230-250 kg, optical rotation ≥ -55°.

[0019] 6. After centrifugation, put the mother liquor into the output D-(-)-p-hydroxyphenylglycine o-toluenesulfonate equal weight of DL-p-hydroxyphenylglycine o-toluenesulfonate, after heating up and completely...

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Abstract

The invention relates to a technology for splitting DL-p-hydroxyphenylglycine-o-toluenesulfonate, which belongs to the field of the production of pharmaceutical and chemical intermediates and relates to a technology for splitting a compound having the following structure. The splitting acceptability of the traditional DL-p-hydroxyphenylglycine-o-toluenesulfonate is not more than 85 percent, unacceptable materials need to be processed again, the labor intensity of workers is enhanced, and low yield, high production cost and market competitive force deficiency are caused. The defects are overcome in the invention; by adopting the method, the splitting acceptability can reach more than 95 percent, and the yield is improved to more than 98 percent from the original 91 percent; and not only the labor intensity of the workers is lightened, but also the production cost is greatly reduced due to the improvement of the yield, thus two purposes are achieved with one technology. Because the production cost is reduced, the market competitive force is improved.

Description

[0001] Field [0002] The invention belongs to the field of production of pharmaceutical and chemical intermediates, and is a technology for splitting compounds with the following structure: [0003] [0004] The chemical name is DL-p-hydroxyphenylglycine o-toluenesulfonate. After resolution, purification and hydrolysis, D-p-hydroxyphenylglycine and L-p-hydroxyphenylglycine can be obtained, which are important intermediates for the synthesis of new anticancer drugs. And the side chain of semi-synthetic amoxicillin and cefadroxil. Background technique [0005] Before the present invention, the resolution rate of DL-p-hydroxyphenylglycine o-toluenesulfonate was not more than 85%, and unqualified materials had to be re-cooked, which not only increased the labor intensity of workers, but also resulted in low yield and high production cost. , no market competitiveness. The present invention overcomes the above-mentioned shortcoming, adopts this method and can make the pass rat...

Claims

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Application Information

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IPC IPC(8): C07C229/36C07C227/34
Inventor 谢建中
Owner HENAN NEWLAND PHARMA
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