Method for refining clopidogrel hydrogen sulfate

A technology of clopidogrel bisulfate and crude clopidogrel bisulfate, which is applied in the direction of organic chemistry, can solve the problems of cumbersome operation steps and unfavorable large-scale production, and achieve the effects of simple post-processing, convenient operation and high yield

Active Publication Date: 2014-07-16

ZHEJIANG HUAHAI PHARMACEUTICAL CO LTD

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AI-Extracted Technical Summary

Problems solved by technology

CN102391283 Tao Lingang and others have reported the refining of clopidogrel hydrogen sulfate, but neutral alumina chromatographic column i...

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Abstract

The invention provides a method for refining clopidogrel hydrogen sulfate. The method comprises the steps of adding a clopidogrel hydrogen sulfate crude product to be purified to mixed solvents, firstly stirring and heating the mixture until the solution is clear, and then cooling and crystallizing the solution, thus obtaining clopidogrel hydrogen sulfate. Obtained clopidogrel hydrogen sulfate can be further pulped and dried in organic solvents to obtain high-purity clopidogrel hydrogen sulfate. The refining method provided by the invention is convenient to operate, is simple in after-treatment and especially has an obvious effect on removing the impurity C, namely the enantiomer of clopidogrel hydrogen sulfate. The obtained product has high yield and good purity and is suitable for large-scale industrial production.

Application Domain

Organic chemistry

Technology Topic

SolventAfter treatment +5

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Experimental program(8)

Example Embodiment

[0027] Example 1: 100 g of crude clopidogrel hydrogen sulfate, 10 g of methanol solution and 800 g of acetone solution were added together into a reaction flask, and then the reaction solution was heated to 20° C. After being completely dissolved, the temperature was slowly lowered to 15°C, and off-white crystals were precipitated. The crystals were slurried in acetone solution, filtered, and vacuum-dried at 30°C to obtain white crystals with a yield of 90%, a purity of 99.8%, and mp : 184~186℃, [α] D =55.0°.

Example Embodiment

[0028] Example 2: 100 g of crude clopidogrel hydrogen sulfate, 100 g of methanol solution and 100 g of ethyl acetate solution were added together into a reaction flask, and then the reaction solution was heated to 35°C. After complete dissolution, slowly lower the temperature to -15°C, precipitate off-white crystals, filter with suction, beat the crystals in ethyl acetate solution, filter, and then vacuum dry at 50°C to obtain white crystals with a yield of 87% , with a purity of 99.6%, mp: 184-186°C, [α] D =55.0°.

Example Embodiment

[0029] Example 3: 100 g of crude clopidogrel hydrogen sulfate, 20 g of methanol solution and 300 g of methyl tert-butyl ether solution were added into a reaction flask, and then the reaction solution was heated to 30°C. After completely dissolving, slowly lower the temperature to 5°C to precipitate off-white crystals, filter them with suction, beat the crystals in a solution of methyl tert-butyl ether, filter, and then dry them under vacuum at 60°C to obtain white crystals. 85%, purity 99.7%, mp: 184-186°C, [α] D =55.0°.

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Description & Claims & Application Information

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Classification and recommendation of technical efficacy words

Post-processing is simple
Easy to operate

Method for refining clopidogrel hydrogen sulfate

AI-Extracted Technical Summary

Problems solved by technology

Abstract

Image

Examples

Example Embodiment

Example Embodiment

Example Embodiment

PUM

Description & Claims & Application Information

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