Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Crystal r of esomeprazole sodium salt and its preparation method and use

A technology of esomeprazole sodium salt and esomeprazole is applied to the crystal R of esomeprazole sodium salt and the fields of its preparation and use, and can solve the problems of wet filter cake viscosity, filtration separation and washing difficulties and other problems, to achieve the effect of good stability, easy filtration separation and washing, and good chemical purity

Inactive Publication Date: 2016-01-20
CHONGQING Y S F PHARMA +1
View PDF7 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Because amorphous esomeprazole sodium salt (as shown in formula I) easily absorbs the moisture in the air and deliquesces, thereby brings very big difficulty to filtration separation and washing, and the wet filter cake that separation obtains is viscous , it needs to be dried for a long time, and the moisture content can be qualified

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Crystal r of esomeprazole sodium salt and its preparation method and use
  • Crystal r of esomeprazole sodium salt and its preparation method and use
  • Crystal r of esomeprazole sodium salt and its preparation method and use

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] The preparation a of embodiment 1 esomeprazole sodium salt crystal R

[0054] At room temperature, 54.7g (0.16mol) of esomeprazole oil was dissolved in 69ml of methanol, and at -10°C, 125ml of methanol solution containing 10.4g (0.26mol) of sodium hydroxide was added dropwise, and stirred at 25°C for 1 After 1 hour, it was cooled to 0° C., and a white solid precipitated out. It was suction-filtered, washed with ice methanol, washed with isopropyl ether, and dried under reduced pressure in vacuo to obtain 34.3 g of a white solid. Yield: 65.8%, ee value 100%, decomposition point 220±2°C.

Embodiment 2

[0055] Preparation a of the crystal R of embodiment 2 esomeprazole sodium salt

[0056] At room temperature, dissolve 46.6g (0.13mol) of esomeprazole oil in 64ml of methanol, and at 0°C, add dropwise 105ml of methanol solution containing 23.8g (0.44mol) of sodium methoxide, and stir at 30°C for 20 hours , cooled to -30°C, a white solid was precipitated, filtered with suction, washed with ice methanol, washed with isopropyl ether, and dried under reduced pressure in vacuo to obtain 26.2 g of a white solid. Yield: 65.8%, ee value 100%, decomposition point 220±2°C.

Embodiment 3

[0057] Preparation a of embodiment 3 esomeprazole sodium salt crystal R

[0058] At room temperature, dissolve 5.2 g (0.015 mol) of esomeprazole oil in 500 ml of methanol, and at -30 ° C, dropwise add 100 ml of ethanol solution containing 3.0 g (0.075 mol) of sodium hydroxide, and stir at 25 ° C for 10 hours After cooling to -10°C, a white solid precipitated out, which was suction filtered, washed with ice methanol, washed with isopropyl ether, and dried under reduced pressure in vacuo to obtain 1.2 g of a white solid. Yield: 21.0%, ee value is 100%, decomposition point is 220±2°C.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
decomposition temperatureaaaaaaaaaa
lengthaaaaaaaaaa
Login to View More

Abstract

The invention discloses a crystal R of sodium esomeprazole, a preparation method and a purpose thereof. The crystal R provided by the invention is a novel crystal form of the sodium esomeprazole, has a good chemical purity (without isomer, and an ee value being 100 %) and physical stability, and is easy to filter, separate and wash. The crystal is low in moisture content (1.31 %) after being vacuum-dried for 5 minutes at 35 DEG C, and good in stability. Crystal samples of the sodium esomeprazole provided by the invention in different batches are subjected to an HPLC detection, and has a purity of more than 99.8 %, with no isomers being detected. The preparation method provided by the invention can prepare the crystal R with stable and consistent performances in each batch, and is simple in preparation technology and good in repeatability.

Description

technical field [0001] The invention relates to a crystal R of esomeprazole sodium salt, a preparation method and application thereof. Background technique [0002] Esomeprazole as the S-configuration isomer of omeprazole, namely (-)-5-methoxy-2-[[(4-methoxy-3,5-dimethyl-2 -pyridyl)-methyl]sulfinyl]-1H-benzimidazole. [0003] [0004] Formula I [0005] Esomeprazole (preparation method: Tetrahedron: Asymmetry11, 3819-3825), as a proton pump inhibitor, can be used to treat diseases related to gastric acid; at the same time, it has improved pharmacokinetics as a single isomer of omeprazole Kinetic and metabolic properties, resulting in an improved therapeutic spectrum. [0006] Because amorphous esomeprazole sodium salt (as shown in formula I) easily absorbs the moisture in the air and deliquesces, thereby brings very big difficulty to filtration separation and washing, and the wet filter cake that separation obtains is viscous , It needs to be dried for a long time bef...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07D401/12A61K31/4439A61P1/04
Inventor 唐超隋强刘帅时惠麟
Owner CHONGQING Y S F PHARMA
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com