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A kind of refining method of l crystal form eplerenone

A technology for eplerenone and a refining method, which is applied in the refining field of L crystal form eplerenone, can solve the problems of high equipment requirements, high temperature, difficult to achieve residual solvent, etc., and achieves good impurity removal effect and simple operation. Effect

Active Publication Date: 2016-06-01
HEFEI JIUNUO MEDICAL TECH
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  • 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

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  • A kind of refining method of l crystal form eplerenone
  • A kind of refining method of l crystal form eplerenone
  • A kind of refining method of l crystal form eplerenone

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%.

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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

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Application Information

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