Method for purifying urapidil by anti-solvent recrystallization method

An anti-solvent recrystallization and urapidil technology, applied in the direction of organic chemistry, can solve the problems of low yield and long crystallization time, and achieve the effect of high yield, rapid precipitation and easy control of conditions

Inactive Publication Date: 2011-12-07
HENAN FUREN MEDICAL TECH DEV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When using these solvents to carry out urapidil recrystallization, there are long crystallization time, the defect that yield is low, therefore, a kind of purification method that can improve recrystallization yield and can complete operation process fast remains to be developed

Method used

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  • Method for purifying urapidil by anti-solvent recrystallization method
  • Method for purifying urapidil by anti-solvent recrystallization method
  • Method for purifying urapidil by anti-solvent recrystallization method

Examples

Experimental program
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Effect test

Embodiment 1

[0019] Add 5g of urapidil (purity 96.16%) to 15ml of dichloromethane, heat it at 40°C to dissolve it, filter it while hot, and add the filtrate to the anti-solvent 30ml of ethyl formate at 5ml / min, and quickly When white turbidity appeared, it was left to stand for 0.5 h, filtered under reduced pressure, and the obtained solid was dried under vacuum at room temperature to obtain 4.87 g of urapidil with a yield of 97.4% and a purity of 99.98%.

[0020] The purity of the product was detected by Shimadzu LC-10ATvp high performance liquid chromatograph (SPD-10ATvp detector).

[0021] Detection method: National standard for new drug conversion [WS1-(X-116)-2003Z].

[0022] attached figure 1 The results of HPLC analysis of urapidil standard are as follows:

[0023] attached figure 2 The HPLC analysis results of Urapidil before the anti-solvent recrystallization of Experimental Example 1 are as follows:

[0024] attached image 3 The HPLC analysis results of Urapidil aft...

Embodiment 2

[0027] Add 5g of urapidil (purity 96.16%) to 15ml of DMSO, heat it at 45°C to dissolve it, filter it while hot, and the obtained filtrate is added to 50ml of petroleum ether at a rate of 10ml / min, and white turbidity quickly appears. Set for 0.5 h, filter under reduced pressure, and vacuum dry the obtained solid at room temperature to obtain 4.79 g of urapidil with a yield of 95.8% and a purity of 99.98%.

Embodiment 3

[0029] 5g of urapidil (purity 96.16%) was added to 15ml of THF, heated at 45°C to dissolve it, filtered while hot, and the obtained filtrate was added to the anti-solvent 30ml of ethyl acetate and 10ml of petroleum ether at a rate of 15ml / min, White turbidity quickly appeared, left standing for 0.5 h, filtered under reduced pressure, and the obtained solid was vacuum-dried at room temperature to obtain 4.67 g of urapidil with a yield of 93.4% and a purity of 99.93%.

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Abstract

The invention discloses a method for purifying urapidil, in particular to a method for purifying urapidil with a counter solvent recrystallization method, belonging to the field of purification of compounds. The method is implemented by the following steps of: adding urapidil of which the purity is over 96 percent into an organic solvent; heating and dissolving; performing suction filtration; pouring the filtrate into a counter solvent; standing; performing suction filtration under reduced pressure; and performing vacuum drying to obtain the urapidil. The method has the advantages of simpleness in operation, short time needed for precipitating a product, higher yield of the obtained urapidil than that of the prior art, and purity of over 99.82 percent (HPLC (High Performance Liquid Chromatography)); and the method is extremely suitable for industrial production.

Description

technical field [0001] The invention relates to a method for purifying urapidil, in particular to a method for purifying urapidil by using an anti-solvent recrystallization method, and belongs to the field of compound purification. Background technique [0002] Urapidil (Urapidil) is phenylazine substituted uracil, its chemical name is 6-[[3-[4-(2-methoxyphenyl)-1-piperazinyl]-propyl]-amino] -1, 3-Dimethyl-2, 4(1H, 3H)-pyrimidinedione, English name is 6-[[3-[4-(2-methoxyphenyl)-1-piperazinyl]propyl]amino]-1 ,3-dimethyl-2, 4(1H, 3H)-pyrimidinedione, the structural formula is: [0003] [0004] The trade names of urapidil hydrochloride are vasodine, Ebrantil and lixidine. Its mechanism of action is 1 Receptor blockers and weaker beta-blockers have both peripheral and central antihypertensive effects. Peripheral major block alpha 1 receptors, and excite central 5-HT 1A Receptors, thereby reducing the sympathetic feedback regulation of the medulla oblongata cardiovascul...

Claims

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Application Information

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IPC IPC(8): C07D239/545
Inventor 陈水库李雯马晓青朱松林姬力莎朱成功杨雷黄占海陈永强
Owner HENAN FUREN MEDICAL TECH DEV
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