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Preparation of mitiglinide calcium and its quality control method

A mitiglinide calcium and quality technology, applied in the field of preparation and detection of hypoglycemic drugs, can solve problems such as harsh conditions, unsuitable for industrial production, and complex synthetic routes

Inactive Publication Date: 2008-12-10
天津汉康医药生物技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Drugs of the Future 2000, 25 (10) also introduced a method for preparing mitiglinide calcium. These methods have complicated synthetic routes, low yield, inconvenient operation and harsh conditions, and are not suitable for industrial production

Method used

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  • Preparation of mitiglinide calcium and its quality control method
  • Preparation of mitiglinide calcium and its quality control method
  • Preparation of mitiglinide calcium and its quality control method

Examples

Experimental program
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Effect test

Embodiment 1

[0084] Step 1. Synthesis of cis-cyclohexyl-1,2-dicarboximide

[0085] Dissolve cyclohexene-1,2-dicarboximide (30g, 199mmol) in methanol (1000ml), add 10% Pd / C (0.3g), vent hydrogen, and stir at room temperature for 28 hours until no hydrogen absorption is complete. After filtration, the filtrate was concentrated to obtain white crystals. The mass is: 30.2g; the yield is: 99.3%.

[0086] Step 2. Synthesis of cis-hexahydroisoindole

[0087] Lithium tetrahydroaluminum (18.6g, 490mmol) was added to dry tetrahydrofuran (150ml), and a solution of cis-cyclohexyl-1,2-dicarboximide (30g, 196mmol) in tetrahydrofuran (500ml) was added dropwise with stirring The rate of dropping is to keep the tetrahydrofuran solution refluxing slightly. After all the addition, the reaction solution was refluxed for 30 hours, cooled, and a small amount of water was added to decompose the excess lithium aluminum tetrahydrogen. The resulting precipitate was filtered, the filtrate was concentrated, and the resid...

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Abstract

The invention relates to a preparation and quality control method of Mitiglinide Calcium comprising steps: 1,synthesis of cis- cyclohexyl-1,2-dimethylacid imide; 2,synthesis of cis-hexa-hydrogen isoindole; 3,synthesis of alpha-benzyldiethyl malonate; 4,synthesis of benzylsuccinic acid; 5,S- benzylsuccinic acid methylbenzylamine salt; 6,synthesis of s- benzylsuccinic acid; 7,synthesis of (2S)-2- benzyl-3-(cis-hexa-hydrogen isoindole-2- carbonyl) propanoic acid; 8,synthesis of Mitiglinide Calcium; 9,purity of Mitiglinide Calcium. This invention also contains the method for quality control of Mitiglinide Calcium comprising steps: watching deseription, messureing specific rotation, authenticating, checking, content messureing for Mitiglinide Calcium.

Description

Technical field [0001] The invention relates to a method for preparing and detecting a blood glucose lowering drug, in particular to a method for preparing and quality control of mitiglinide calcium. Background technique [0002] Diabetes is a common and frequently-occurring disease, and the number of its patients is increasing rapidly with the improvement of people's living standards, aging of the population, changes in lifestyles and advances in diagnostic technology. According to relevant data from the WHO, the prevalence, disability, mortality, and damage of diabetes ranks the third among non-communicable diseases. It has become the first serious threat to human health after cardiovascular and cerebrovascular diseases and tumors. Three major diseases, this disease not only brings great pain to the patients, the quality of life is greatly affected, but also brings a heavy economic burden to the society. [0003] At present, the oral hypoglycemic agents clinically used to treat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D209/08A61K31/404A61P3/10G01N21/82G01N21/35G01N33/02G01N21/3563
Inventor 严洁
Owner 天津汉康医药生物技术有限公司
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