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Preparation method of dex-ilaprazole potassium salt mother liquor, dex-ilaprazole and preparation method thereof

A technology of dextro-ilaprazole potassium salt and ilaprazole potassium salt, applied in the field of dextro-ilaprazole and preparation thereof, can solve the problems of being unsuitable for industrialized production, harsh experimental conditions, long time-consuming and the like, and achieves The process method is simple and easy to implement, the e.e value is stable, and the effect of high e.e value

Active Publication Date: 2020-03-31
LIVZON PHARM GRP INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method takes a long time, the experimental conditions are relatively harsh, and it needs to be placed overnight at low temperature, which is not suitable for industrial production

Method used

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  • Preparation method of dex-ilaprazole potassium salt mother liquor, dex-ilaprazole and preparation method thereof
  • Preparation method of dex-ilaprazole potassium salt mother liquor, dex-ilaprazole and preparation method thereof
  • Preparation method of dex-ilaprazole potassium salt mother liquor, dex-ilaprazole and preparation method thereof

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Experimental program
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preparation example Construction

[0024] A kind of preparation method of dex-ilaprazole provided by the embodiment of the present invention comprises the following steps:

[0025] Preparation of S1, dextroilaprazole potassium salt mother liquor

[0026] The potassium salt of ilaprazole and the first organic solvent are mixed and beaten, and the solid-liquid separation is carried out to obtain the potassium salt mother liquor of ilaprazole enriched in the dextro-isomer of the potassium salt of ilaprazole. Through the selection of the organic solvent, the ilaprazole potassium salt enters the liquid phase, and the mother liquor is separated by filtration, so that the e.e. value of the ilaprazole potassium salt in the mother liquor is significantly improved, and the result has high stability.

[0027] What needs to be added is that the potassium salt of dex-ilaprazole cannot be replaced by other raw materials, such as sodium salt of dex-ilaprazole, and dex-ilaprazole with high e.e value cannot be obtained by using...

Embodiment 1

[0044] The present embodiment provides a kind of preparation method of dex-ilaprazole, it comprises the following steps:

[0045] Take 2.00 g of (+)-ilaprazole potassium salt (e.e 79.4%), add 24 ml of dichloromethane, and perform beating at 20° C. for 4 h. Finally, filter out the filtrate, spin the filtrate to dry, add 10ml of water, 8ml of methanol and stir evenly, then add dilute acetic acid to adjust the pH to 8.0, add dichloromethane for extraction twice, add 10mL each time, combine the organic phases, add anhydrous magnesium sulfate, Dry triethylamine for 30mins, filter, spin the filtrate, add 16mL isopropanol, stir at 20-30°C for 1.5h, filter to obtain (+)-ilaprazole solid, weigh 0.79g after vacuum drying, measure e.e The value is 99.3%, the product yield in the above (+)-ilaprazole potassium salt mother liquor is measured to be 49%, and the solid yield of (+)-ilaprazole in the final product is 79.8%.

[0046] It should be noted that the calculation method of (+)-ilapra...

Embodiment 2

[0050] The present embodiment provides a preparation method of dex-ilaprazole, which comprises the following steps: take (+)-ilaprazole potassium salt (e.e 79.4%) 2.00g, add 24ml of dichloromethane, and carry out at 30°C Beat for 1h. Finally, filter out the filtrate, spin the filtrate to dry, add 10ml of water, 8ml of methanol and stir evenly, then add diluted acetic acid to adjust the pH to 8.0, add dichloromethane for extraction twice, each time adding 10mL, combine the organic phase, add anhydrous magnesium sulfate, Dry triethylamine for 30mins, filter, spin the filtrate, add 16mL acetonitrile, stir at 20-30°C for 1.5h, filter to obtain (+)-ilaprazole solid, weigh 0.75g after vacuum drying, and measure e.e. 99.0%, the measured product yield in the above (+)-ilaprazole potassium salt mother liquor is 51%, and the solid yield of (+)-ilaprazole is 81.3%.

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Abstract

The invention discloses a preparation method of a dextral ilaprazole potassium salt mother liquor, dextral ilaprazole and a preparation method thereof, and relates to pharmaceutical intermediates. Thepreparation method of the dextral ilaprazole potassium salt mother liquor comprises: mixing a dextral ilaprazole potassium salt to be purified and a first organic solvent, performing beating to makean ilaprazole potassium salt dextral isomer enters into the mother liquor, and performing solid-liquid separation to obtain the mother liquor enriched with the dextral ilaprazole potassium salt. The above mother liquor is used as a raw material to react with a reaction used acid to form dextral ilaprazole, the assisted dissolution action of water and a second organic solvent is used to prevent theprecipitation of dextral ilaprazole, and then the purification of dextral ilaprazole is carried out. The obtained dextral ilaprazole has a high e.e value, the e.e value is not affected by an e.e value of the dextral ilaprazole potassium salt, the e.e value of the product is stable, and the difference between batches is small.

Description

technical field [0001] The invention relates to the technical field of pharmaceutical intermediates, and in particular to a kind of dex-ilaprazole and a preparation method thereof. Background technique [0002] Ilaprazole is a novel proton pump inhibitor for the treatment of duodenal ulcer, gastric ulcer and erosive esophagitis. Ilaprazole contains a chiral center and is a racemic mixture of two single enantiomers, the R and S enantiomers. Disclosed in CN101098867A is the preparation method of single enantiomer of ilaprazole, and animal experiments show that the optical isomers of ilaprazole, i.e. D- or L-ilaprazole and its racemate, are more effective in treating hyperacidity. It has more excellent therapeutic effects in multiple related diseases. [0003] Patent CN1098261C discloses a purification method for several compounds with high enantiomeric content of prazoles. The racemate is selectively crystallized with a solvent, and the solvent in the solution is evaporated ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D401/14
CPCC07B2200/07C07D401/14
Inventor 谢诗琳王涛侯雪梅李普成崔艳南成彩华谌红丹谭文绘赵海丽吴小红陈乐平莫雅婷温弘鲍靖刘学明
Owner LIVZON PHARM GRP INC
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