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Refining method of tiopronin

A tiopronin, refining and purification technology, applied in the field of medicine and chemical industry, can solve the problems of low product purity, long production cycle, difficult process control, etc., and achieve the effect of simple refining process and high yield

Inactive Publication Date: 2013-04-24
GUANGDONG XIANQIANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This new way of making drugs has several technical benefits: it allows for better control over their quality; efficient production with ease compared to existing methods that use expensive chemicals or complicated processes like extraction from plants.

Problems solved by technology

This patented technical problem addressed in this patents relates to improving methods or techniques for producing tertonosynthesis antagonists such as titaprons while reducing their associated safety concerns due to its lower toxiant property compared to existing drugs like cytotecan.

Method used

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  • Refining method of tiopronin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Put 80g of crude product tiopronin (purity 96.8%) in a 1000ml four-neck flask, add 240ml of ethyl acetate and 40ml of acetone, heat up and reflux for 0.5 hours, stir and cool down to room temperature 30°C, keep warm for 0.5 hours, continue to cool down to 0- 5°C, stir and keep warm for 2 hours, filter, rinse the wet product with a small amount of n-hexane at 0-5°C, dry the sample in vacuum at 45°C for 6-8 hours, and obtain 65.6g of refined sample, yield 82%, purity 98.8% , the single impurity content is in line with the State Food and Drug Administration Drug Trial Standard (YBH 12042005).

Embodiment 2

[0029] Put 80g of crude product tiopronin (purity 96.8%) in a 1000ml four-neck flask, add 320ml of ethyl acetate and 40ml of acetone, heat up and reflux for 2 hours, stir and cool down to room temperature 30°C, keep warm for 1 hour, continue to cool down to 0- 5°C, stir and keep warm for 5 hours, filter, rinse the wet product with a small amount of n-hexane at 0-5°C, dry the sample in vacuum at 45°C for 6-8 hours, and obtain 60.3g of refined sample, yield 75.4%, purity 99.1% , the single impurity content is in line with the State Food and Drug Administration Drug Trial Standard (YBH 12042005).

Embodiment 3

[0031] Put 80g of crude product tiopronin (purity 96.8%) in a 1000ml four-neck flask, add 240ml of ethyl acetate and 80ml of acetone, heat up and reflux for 1 hour, stir and cool down to room temperature 30°C, keep warm for 2 hours, continue to cool down to 0- 5°C, stir and keep warm for 8 hours, filter, rinse the wet product with a small amount of n-hexane at 0-5°C, dry the sample in vacuum at 45°C for 6-8 hours, and obtain 63.8g of refined sample, yield 79.7%, purity 99.3% , the single impurity content is in line with the State Food and Drug Administration Drug Trial Standard (YBH 12042005).

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Abstract

The invention relates to the application of a method for refining tiopronin through component solvent. Tiopronin is resolved in mixed solvent of ester solvent and oxazolidinone solvent or mixed solvent of ester solvent, oxazolidinone solvent and aliphatic alkane solvent, and the effect of removing impurities of tiopronin can be achieved through a crystallization procedure; and through the method, the effect of removing the impurity of a-chloro propionyl glycine in tiopronin is remarkable. The method has the advantages that the process procedures are simple, the operation is easy and the product yield is high.

Description

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Claims

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Application Information

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Owner GUANGDONG XIANQIANG PHARMA
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