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Liquid chromatography detection method for synthesizing Eldecalcitol intermediate

A technology of idecalcitol and liquid chromatography, which is applied in the field of liquid chromatography detection of synthetic idecalcitol intermediates, can solve the problem that it is difficult to monitor the reaction of two starting materials at the same time, the price is expensive, and the ELD-2 There is a big difference in UV absorption from SM2, etc.

Active Publication Date: 2020-10-30
大连美创药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, ELD-2 and SM2 are expensive, and the UV absorption of ELD-2 and SM2 is quite different. It is difficult to monitor the reaction of the two starting materials at the same time with the existing high-performance liquid chromatography detection method. Therefore, a reasonable intermediate control method should be developed. Monitoring the synthesis process can greatly reduce enterprise R&D costs and improve R&D efficiency

Method used

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  • Liquid chromatography detection method for synthesizing Eldecalcitol intermediate
  • Liquid chromatography detection method for synthesizing Eldecalcitol intermediate
  • Liquid chromatography detection method for synthesizing Eldecalcitol intermediate

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Embodiment 1

[0028] A liquid chromatography detection method for synthesizing idecalcitol intermediate, the liquid chromatography detection method is:

[0029] The analytes include: (1R,3aR,7aR)-7a-methyl-1-((R)-6-methyl-6-((triethylsilyl)oxy)heptan-2-yl) Cynyl-4H-inden-4-one, ((Z)-2-((3R,4R,5R)-3,5-bis((tert-butyldimethylsilyl)oxy)-4-(4 -((tert-butyldimethylsilyl)oxy)butoxy)-2-methylenecyclohexyl)ethyl)diphenylphosphine oxide, ((1R,2R,3R,Z)-2- (3-((tert-butyldimethylsilyl)oxy)propoxy)-5-(2-((1R,3aS,7aR,E)-7a-methyl-1-((R)- 6-Methyl-6-((triethylsilyl)oxy)heptan-2-yl)octyl-4H-indene-4-ylidene)ethylene)-4-methylenecyclohexyl alkane-1,3-diyl)bis(oxy)tert-butyldimethylsilane);

[0030] The conditions of liquid chromatography are:

[0031] The stationary phase is: Daicel OD-RH chromatographic column, the particle size of the spherical silica gel is 5 μm, the length of the chromatographic column is 150 mm, and the inner diameter of the chromatographic column is 4.6 mm;

[0032] Column tempe...

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Abstract

The invention relates to a liquid chromatography detection method for synthesizing an Eldecalcitol intermediate, which belongs to the field of analytical chemistry. The conditions of the liquid chromatography are as follows: a stationary phase is silica gel of which the surface is coated with cellulose-tri(3, 5-dimethylphenyl carbamate); the mobile phases are acetonitrile and water, and gradient elution is carried out; the detector is an ultraviolet detector, and is used for detecting ELD-2 under 197 nm and detecting SM2 and ELD-3 under 210 nm.

Description

technical field [0001] The invention relates to a liquid chromatography detection method for synthesizing an idecalcitol intermediate, belonging to the field of analytical chemistry. Background technique [0002] Idecalcitol is an activated vitamin D3 derivative with bone formation function developed by Chugai Pharmaceutical Co., Ltd., mainly used for the treatment of osteoporosis. Its chemical name is (5Z,7E)-(1R,2R,3R)- 2-(3-Hydroxypropoxy)-9,10-secocholesta-5,7,10(19)-triene-1,3,25-triol, the structural formula is as formula (I): [0003] [0004] ((1R,2R,3R,Z)-2-(3-((tert-butyldimethylsilyl)oxy)propoxy)-5-(2-((1R,3aS,7aR,E) -7a-Methyl-1-((R)-6-methyl-6-((triethylsilyl)oxy)heptane-2-yl)octyl-4H-indene-4-ylidene ) Ethylene)-4-methylenecyclohexane-1,3-diyl) bis(oxygen) tert-butyldimethylsilane) is an important intermediate for the synthesis of idecalcitol, and its structural formula is as follows (Ⅱ): [0005] [0006] Formula (II) is obtained through (1R,3aR,7aR)...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/34
CPCG01N30/02G01N30/06G01N30/34
Inventor 梁晓云贾志强
Owner 大连美创药业有限公司