Method for purifying 3-(2-cyclopentyl-2-hydroxy-2-phenylethoxy) quinuclidine and preparing penehyclidine hydrochloride

A technology of phenylethoxy and purification method, which is applied in the field of purification of 3-quinuclidin and preparation of penhyclidine hydrochloride, can solve the problem of lack of impurity removal and purification process of the target product, low purity and yield, and product Complicated operation and other issues, to achieve the effect of low cost, simple purification method, and easy-to-obtain raw materials
CN111004232AActive Publication Date: 2020-04-14北京鑫开元医药科技有限公司
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
北京鑫开元医药科技有限公司
Publication Date
2020-04-14

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Abstract

The invention provides a method for purifying 3-(2-cyclopentyl-2-hydroxy-2-phenylethoxy) quinuclidine and preparing penehyclidine hydrochloride. The method comprises the following steps: (1) mixing 3-quinuclidinol with a dimethyl sulfoxide solution, and reacting with sodium hydride and a 1,1-phenyl amyl oxirane solution; (2) adding purified water and ethyl acetate to carry out extraction, collecting the organic phase, washing, carrying out back extraction with a hydrochloric acid solution, and collecting the water layer; (3) adjusting the pH value of the water layer to 5-7, washing the water layer by ethyl acetate, adjusting the pH value to 9-12 again, extracting the water layer by ethyl acetate, and collecting the organic phase; and (4) filtering, and carrying out reduced pressure concentration to obtain 3-(2-cyclopentyl-2-hydroxy-2-phenylethoxy) quinuclidine oil. According to the method, by separating and purifying 3-(2-cyclopentyl-2-hydroxy-2-phenylethoxy) quinuclidine, the yield and quality of a target product are improved, and a penehyclidine hydrochloride finished product with a high yield and high purity is obtained through one-step salifying crystallization.
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Description

technical field

[0001] The invention relates to the technical field of medicinal chemistry, in particular to a method for purifying 3-(2-cyclopentyl-2-hydroxy-2-phenylethoxy)quinuclidine and preparing penhyclidine hydrochloride. Background technique

[0002] Penehyclidine hydrochlordie is a new anticholinergic drug developed by the Academy of Military Medical Sciences in my country. The chemical name is 3-(2-cyclopentyl-2-hydroxy-2-phenylethoxy)quinuclidine hydrochloride, which is the bioisostere analog of diphenylglycolic acid-3-quinuclidinol things. Studies have shown that penehyclidine hydrochloride is a selective anticholinergic drug. At present, vardenafil hydrochloride has been successfully used in the clinical treatment of organophosphorus pesticide poisoning, with high antitoxic potency, long-lasting antitoxic effect and small adverse effects. At the same time, penehyclidine hydrochloride has anticholinergic effects on gastrointestinal diseases, eye diseases, resp...

Claims

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