A kind of assay method of r-3-quinuclidinol optical purity

A technology of optical purity and determination method, applied in the field of medicine and chemical industry, can solve the problems of difficult chiral chromatographic separation, lack of groups, inapplicability, etc., and achieve the effect of good peak purity and enhanced identification ability.
CN104133018BActive Publication Date: 2015-12-02JINAN ASIA PHARMA TECH
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
JINAN ASIA PHARMA TECH
Publication Date
2015-12-02

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Abstract

The invention belongs to the technical field of pharmaceutical chemical engineering, and in particular relates to a method for measuring the optical purity of (R)-3-quinuclidinol. The method for measuring the optical purity of (R)-3-quinuclidinol comprises the steps of (a) preparing a sample; (b) preparing a test solution; (c) preparing a chromatographic condition, and performing detection. According to the method, a precolumn derivatization chiral chromatography method is adopted to measure the optical purity of (R)-3-quinuclidinol; specifically, the precolumn derivatization method is used for enabling (RS)-3-quinuclidinol racemate and paratoluensulfonyl chloride to react to generate (RS)-3-quinuclidinol paratoluensulfonyl chloride derivative, namely quinuclidinol 3-paratoluene sulfonate; then the chiral chromatography method is used for measuring the optical purity; therefore, the technical difficulty in measurement of the optical purity of (R)-3-quinuclidinol is creatively solved.
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Description

technical field

[0001] The invention belongs to the technical field of medicine and chemical industry, and in particular relates to a method for measuring the optical purity of R-3-quinuclidinol. Background technique

[0002] The chemical name of (R)-3-quinuclidinol is 1-azacyclo[2.2.2]octane(R)-3-ol, which is a synthetic muscarinic receptor antagonist such as solifenacin, Important intermediates of valtropate, tasalidine, etc., the structural formula of R-3-quinuclidin is as follows: .

[0003] The synthesis of (R)-3-quinuclidinol is to use 3-quinuclidinone as raw material to generate (RS)-3-quinuclidinol through carbonyl reduction, and then obtain (R)-3-quinuclidinol through resolution Niclidinol, the purity of (R)-3-quinuclidinol after resolution is described by measuring the optical rotation and calculating the ee value. The method of measuring the optical rotation to calculate ee has a large error in the determination of the optical purity of (R)-3-quinuclidinol. Fi...

Claims

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