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

L-crystal form eplerenone refining method

A refining method, the technology of eplerenone, applied in the direction of steroids, organic chemistry, etc., can solve the problems of high equipment requirements, high temperature, high energy consumption of drying, etc., and achieve the effect of good impurity removal and simple operation

Active Publication Date: 2015-08-19
HEFEI JIUNUO MEDICAL TECH
View PDF6 Cites 3 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The desolvation temperature of the obtained solvate is greater than 100°C, the drying energy consumption is large, the equipment requirements are high, and the residual solvent is difficult to meet the requirements of the current pharmacopoeia

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
  • L-crystal form eplerenone refining method
  • L-crystal form eplerenone refining method
  • L-crystal form eplerenone refining method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Take 50g of crude eplerenone, add 1.2L of 1,2-dimethoxyethane, reflux to dissolve, filter, transfer the filtrate into a 2L reaction flask, stir and cool down to -5~0℃, stir and crystallize for 10h, filter , and the filter cake was dried under reduced pressure at 50° C. for 6 hours to obtain 42 g of eplerenone in L crystal form. Yield 84%, purity 99.93%.

Embodiment 2

[0039] Take 50g of eplerenone ethanol solvate (containing 2.72% ethanol), add 1.2L of 1,2-dimethoxyethane, reflux to dissolve, filter, transfer the filtrate into a 2L reaction bottle, stir and cool down to -5~ 0°C, stirred and crystallized for 10 h, filtered, and dried the filter cake at 60°C for 6 h to obtain 40 g of eplerenone in L crystal form. Yield 82%, purity 99.97%.

Embodiment 3

[0041] Take 50g of eplerenone chloroform solvate (containing 12.45% chloroform), add 800ml of 1,2-dimethoxyethane and 20ml of chloroform, reflux to dissolve, filter, transfer the filtrate into a 2L reaction bottle, stir and cool down to - Stir and crystallize at 5-0°C for 12 hours, filter, and dry the filter cake at 60°C for 6 hours to obtain 31.5 g of eplerenone in L crystal form. Yield 72%, purity 99.91%.

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

No PUM Login to View More

Abstract

The invention discloses an L-crystal form eplerenone refining method which is as follows: an eplerenone raw product is added into 1, 2-dimethoxy ethane solvent system, heated to dissolve, and filtered, the filtrate is cooled for crystallization, filtration, and drying to obtain L-crystal form eplerenone. The volume percentage of 1, 2-dimethoxy ethane in the 1, 2-dimethoxy ethane solvent system is greater than or equal to 50%. The method is simple in operation, high in yield, low in drying temperature, good in effect of removing impurity, and the purity of the L-crystal form eplerenone is above 99.9% (detected by HPLC), and the single impurity peak is less than 0.1%.

Description

1. Technical field [0001] The invention relates to a method for refining known medicines, in particular to a method for refining eplerenone in L crystal form. 2. Background technology [0002] Eplerenone, the chemical name is (7α,11α,17α)-9,11-epoxy-17-hydroxy-3-oxo-pregna-4-ene-7,21-dicarboxylic acid, γ-lactone, 7-methyl ester, the chemical structural formula is shown in the following formula (I): [0003] [0004] Eplerenone is a selective aldosterone antagonist developed by Pfizer / Pharmacia and first launched in the United States in 2002 under the trade name Inspra. Clinically, it is mainly used for the treatment of hypertension, heart failure and myocardial infarction. [0005] Eplerenone has two main crystalline forms: crystalline form H and crystalline form L, and crystalline form L is selected for preparation. CN100413881C discloses a method for preparing crystal form L of eplerenone. First, the corresponding solvate is prepared by crystallization with a specifi...

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
IPC IPC(8): C07J71/00
CPCC07J71/0015
Inventor 吴标凌林戴根来应阳
Owner HEFEI JIUNUO MEDICAL TECH
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