Method for preparing high purity mitiglinide calcium

A mitiglinide calcium and high-purity technology is applied in the field of preparation of high-purity mitiglinide calcium, can solve the problems of difficult purification, high cost, low yield and the like, and achieves strong controllability, low cost and high purity high effect

Inactive Publication Date: 2008-09-24
BEIJING D VENTUREPHARM TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The mitiglinide calcium synthesized with this compound often has impurities brought in by decomposition products. If the purity of perhydroisoindole cannot meet the requirements, it will directly lead to the purity problem of the final product, and the purification is more difficult.
Low yield and high cost are not conducive to industrial production
[0010] In the existing published report of the method for preparing mitiglinide calcium, there is no mention of using an economical and effective method to prepare high-purity mitiglinide calcium, and there is no report about an effective method for refining the product

Method used

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  • Method for preparing high purity mitiglinide calcium
  • Method for preparing high purity mitiglinide calcium
  • Method for preparing high purity mitiglinide calcium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Under a nitrogen atmosphere, 1.5 L of dichloromethane and 65 g of carbonyldiimidazole were added to a 3 L reaction flask. Cool down to -5-0°C, add 62g of (S)-benzylsuccinic acid (compound of formula II), and keep stirring for 1 hour. Add 49g of perhydroisoindole hydrochloride, keep the temperature for 0.5 hours, and gradually raise the temperature of the reaction system to room temperature, and stir for 2 hours. Adjust to acidity with hydrochloric acid, separate the organic phase, and wash with distilled water. The organic phase was washed with saturated sodium bicarbonate. The aqueous phase was separated, adjusted to acidity with concentrated hydrochloric acid, extracted with dichloromethane, the organic phase was dried over anhydrous sodium sulfate, and the solvent was evaporated to obtain a yellow oil. Add 150ml 95% ethanol and 300ml distilled water, and stir well. Adjust alkalinity with 2M sodium hydroxide solution and stir for 0.5 hours. A mixed solution of 55 g...

Embodiment 2

[0034] Under a nitrogen atmosphere, 1.5 L of dichloromethane and 73 g of sulfoxide diimidazole were added to a 3 L reaction flask. Cool down to -5-0°C, add 62g of (S)-benzylsuccinic acid (compound of formula II), and keep stirring for 1 hour. Add 49g of perhydroisoindole hydrochloride, keep the temperature for 0.5 hours, and gradually raise the temperature of the reaction system to room temperature, and stir for 2 hours. Adjust to acidity with hydrochloric acid, separate the organic phase, and wash with distilled water. The organic phase was washed with saturated sodium bicarbonate. The aqueous phase was separated, adjusted to acidity with concentrated hydrochloric acid, extracted with dichloromethane, the organic phase was dried over anhydrous sodium sulfate, and the solvent was evaporated to obtain a yellow oil. Add 150ml 95% ethanol and 300ml distilled water, and stir well. Adjust alkalinity with 2M sodium hydroxide solution and stir for 0.5 hours. A mixed solution of 55...

Embodiment 3

[0036] Under a nitrogen atmosphere, 1.5 L of N,N-dimethylformamide and 73 g of carbonyldiimidazole were added to a 3 L reaction flask. Cool down to 0-5°C, add 62g of (S)-benzylsuccinic acid (compound of formula II), and keep stirring for 1 hour. Add 49g of perhydroisoindole hydrochloride, keep the temperature for 0.5 hours, and gradually raise the temperature of the reaction system to room temperature, and stir for 2 hours. The reaction solution was poured into distilled water, extracted with dichloromethane, washed with hydrochloric acid until acidic, washed with distilled water, and then washed with saturated sodium bicarbonate. The aqueous phase was separated, adjusted to acidity with concentrated hydrochloric acid, extracted with dichloromethane, the organic phase was dried over anhydrous sodium sulfate, and the solvent was evaporated to obtain a yellow oil. Add 150ml 95% ethanol and 300ml distilled water, and stir well. Adjust alkalinity with 2M sodium hydroxide solution...

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Abstract

The present invention relates to a preparation method of high-purity mitiglinide calcium. A compound shown in the formula II and a compound shown in the formula V react under certain conditions to prepare the compound shown in the formula VI that reacts with calcium chloride to prepare the salt mitiglinide calcium.

Description

technical field [0001] The invention relates to a preparation method of high-purity 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, population aging, changes in lifestyle, and advances in diagnostic techniques. Meglitaide is a novel oral fast-acting postprandial hypoglycemic drug, which is a derivative of carbamoylmethylbenzoic acid. Miglinide Calcium is the third meglitaide drug following Repaglinide and Nateglinide, synthesized by Japan Tachibana Pharmaceutical Co., Ltd., and applied for use in patients with type II diabetes in December 2002 Control postprandial blood sugar. At present, it has been approved by the Japanese pharmaceutical authority, trade name: Glufast . Although my country's economy is developing rapidly and people's living standards are improving day by day, the aging of my country's populat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D209/52
Inventor 杨利民
Owner BEIJING D VENTUREPHARM TECH DEV
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