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Purification method of fexofenadine intermediate

A purification method, hydrogen chloride gas technology, applied in the direction of organic chemistry, etc., can solve the problem of high separation cost and achieve the effect of improving product purity

Active Publication Date: 2013-11-27
启东东岳药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, for the purification of the product, the literature and patents either do not introduce it, or use column chromatography for purification, and the separation cost is very high.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 40g of 4-[1-hydroxyl-4[4-(hydroxydiphenylmethyl)-1-piperidinyl]-butyl]-α,α-dimethylphenylacetic acid methyl ester solution into the 500ml reactor, add Add 100ml of acetonitrile, pass through hydrogen chloride to pH 5, keep the temperature at 15-20°C, and stir for 2 hours. Suction filtration and centrifugation, the filtrate was concentrated under reduced pressure until no material came out (that is, the first solvent was removed by evaporation under reduced pressure), and cooled to 15-20°C. Add 150g of ethyl acetate, stir to dissolve, pass hydrogen chloride to pH 2, keep stirring at 15-20°C for 2 hours, filter and centrifuge to obtain 4-[1-hydroxy-4[4-(hydroxydiphenylmethyl)-1 -Piperidinyl]-butyl]-α,α-Dimethylphenylacetic acid methyl ester hydrochloride.

[0026] Add 300g of dichloromethane into a 500ml three-necked flask, add the 4-[1-hydroxyl-4[4-(hydroxydiphenylmethyl)-1-piperidinyl]-butyl]-α,α-di Methyl methyl phenylacetate hydrochloride was added with saturate...

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PUM

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Abstract

The invention discloses a purification method of a fexofenadine intermediate: 4-[1-hydroxy-4[4-(hydroxydiphenylmethyl)-1-piperidyl]-butyl]-alpha,alpha-dimethylmethylphenylacetate. 4-[1-hydroxy-4[4-(hydroxydiphenylmethyl)-1-piperidyl]-butyl]-alpha, alpha-dimethylmethylphenylacetate and chlorine hydride are subjected to salification in a solvent to effectively remove the impurities and enhance the product purity.

Description

technical field [0001] The present invention relates to fexofenadine intermediate: 4-[1-hydroxy-4[4-(hydroxydiphenylmethyl)-1-piperidinyl]-butyl]-α,α-dimethylbenzene Purification method of methyl acetate. Background technique: [0002] 4-[1-Hydroxy-4[4-(hydroxydiphenylmethyl)-1-piperidinyl]-butyl]-α,α-dimethylphenylacetic acid methyl ester is the preparation of antihistamine The key intermediate of Fexofenadine. [0003] 4-[1-Hydroxy-4[4-(hydroxydiphenylmethyl)-1-piperidinyl]-butyl]-α, the preparation method of α-dimethylphenylacetic acid methyl ester is in US4254129, WO9833789, WO9321156 and [0004] It has been reported in many patents such as CN1986530. However, for the purification of the product, the literature and patents either do not introduce it, or use column chromatography to purify, and the separation cost is very high. Contents of the invention [0005] The object of the present invention is to provide a 4-[1-hydroxyl-4[4-(hydroxydiphenylmethyl)-1-piperid...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D211/34
Inventor 龙中柱刘星宇潘天健蔡水洪杨小宝
Owner 启东东岳药业有限公司