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Urapidil hydrochloride crystal form and preparation method thereof

A technology of urapidil hydrochloride and crystal form, which is applied in the field of medicine and can solve problems such as the preparation of urapidil hydrochloride crystal form.

Pending Publication Date: 2020-05-08
LUOXIN PHARM SHANGHAI CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] There is no report on the preparation of urapidil hydrochloride crystal form so far

Method used

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  • Urapidil hydrochloride crystal form and preparation method thereof
  • Urapidil hydrochloride crystal form and preparation method thereof
  • Urapidil hydrochloride crystal form and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0055] The preparation of embodiment 1 urapidil hydrochloride crystal form

[0056] In a 250ml three-neck flask equipped with a reflux condenser, add 160ml of absolute ethanol and 8.1g of refined urapidil, and heat to 60°C with stirring, but it cannot be clarified. Slowly add 3mol / L HCl / MeOH solution dropwise, so that the pH of the reaction solution is between 1-2 with a precision pH meter. At this time, the system is completely clear, continue to stir and keep warm for 1 hour, and slowly cool down to between 25-30°C , stirred at room temperature for about 2 hours, filtered, the filter cake was washed twice with 50ml of absolute ethanol, and the solid was dried in vacuo at 40°C to obtain 7.1g of product, yield: 89.6%, purity > 99% by HPLC, simplex < 0.05%, Product urapidil: HCl=1:1.12.

Embodiment 2

[0057] The preparation of embodiment 2 urapidil hydrochloride crystal form

[0058] In a 250ml three-neck flask equipped with a reflux condenser, add 160ml of absolute ethanol and 8.1g of refined urapidil, and heat to 60°C with stirring, but it cannot be clarified. Slowly add 3mol / L HCl / MeOH solution dropwise, so that the pH of the reaction solution is measured between 2-3 with a precision pH meter. At this time, the system is completely clear, continue to stir and keep warm for 1 hour, and slowly cool down to between 25-30°C , stirred at room temperature for about 2 hours, filtered, the filter cake was washed twice with 50ml of absolute ethanol, and the solid was dried in vacuo at 40°C to obtain 6.2g of product, yield: 75.8%, purity > 99% by HPLC, simplex < 0.05%, Product urapidil: HCl=1:1.2.

Embodiment 3

[0059] The preparation of embodiment 3 urapidil hydrochloride crystal form

[0060]In a 250ml three-neck flask equipped with a reflux condenser, add 165ml of absolute ethanol and 16.2g of refined urapidil, and heat to 60°C with stirring, but it cannot be clarified. Slowly add 3mol / L HCl / MeOH solution dropwise, so that the pH of the reaction solution is measured between 3-4 with a precision pH meter. At this time, the system is completely clear, continue to stir and keep warm for 1 hour, and slowly cool down to between 25-30°C , stirred at room temperature for about 2 hours, filtered, and the filter cake was washed twice with 50ml of absolute ethanol, and the solid was dried in vacuo at 40°C to obtain 15.6g of product, yield: 91.2%, purity > 99% by HPLC, simplex < 0.03%, Product urapidil: HCl=1:1.09.

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Abstract

The invention relates to an urapidil hydrochloride crystal form and a preparation method thereof, specifically to an urapidil hydrochloride crystal form, wherein the X-ray powder diffraction pattern measured by using Cu-Kalpha shows that the crystal form has characteristic diffraction peaks at the following 2[theta] angles: 9.115+ / -0.2 DEG, 15.708+ / -0.2 DEG, 16.203+ / -0.2 DEG, 17.899+ / -0.2 DEG, 18.331+ / -0.2 DEG, 18.904+ / -0.2 DEG, 22.100+ / -0.2 DEG, and 24.294+ / -0.2 DEG.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a crystal form of urapidil hydrochloride and a preparation method thereof. Background technique [0002] Urapidil hydrochloride (urapidil hydrochloride, chemical name 6-[[3-[4-(2-methoxyphenyl)-1-piperazinyl]propyl]amino]-1,3-dimethyl-2 ,4(1H,3H)pyrimidinedione hydrochloride) is a compound having the following chemical structure: [0003] [0004] The compound has both peripheral and central hypotensive effects. Peripheral mainly blocks the post-synaptic α1 receptors, causing vasodilation to significantly reduce peripheral resistance. At the same time, it also has a weak presynaptic α2 blocking effect, blocking the vasoconstrictive effect of catecholamines; the central effect is mainly through stimulating the 5-hydroxytryptamine-1A (5-HT1a) receptor, reducing the sympathetic feedback regulation of the medullary cardiovascular center. pressure. [0005] Clinica...

Claims

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Application Information

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IPC IPC(8): C07D239/545A61P9/12A61P9/04
CPCC07D239/545A61P9/12A61P9/04C07B2200/13
Inventor 唐伟高风明杨文谦王铁林
Owner LUOXIN PHARM SHANGHAI CO LTD
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