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Urapidil impurity compound, preparation method and application thereof

A technology of uradil and uradil hydrochloride, applied in organic chemistry, measuring devices, instruments, etc., can solve problems such as inability to carry out effective quality control, and achieve the effects of improved quality standards, high purity, and good product quality

Pending Publication Date: 2020-12-18
燃点(南京)生物医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Aiming at the problem that there may be a potential impurity in uradil or uradil hydrochloride in the prior art, and effective quality control cannot be carried out, one of the purposes of the invention is to provide a kind of uradil impurity compound, which can be used as uradil The reference substance for the quality control of uradil or urapidil hydrochloride raw materials, which helps to obtain higher quality products

Method used

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  • Urapidil impurity compound, preparation method and application thereof
  • Urapidil impurity compound, preparation method and application thereof
  • Urapidil impurity compound, preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0051] This example prepares a kind of urapidil impurity compound, the preparation method of this urapidil impurity compound is as follows:

[0052] Add 10 g of urapidil, 20 mL of 95% ethanol, and 20 mL of water into the pressure reaction vessel, remove the air in the reaction vessel with carbon dioxide gas, pass the carbon dioxide gas to the set pressure of 60 psi, and keep the temperature at 60°C for 12 hours. After the reaction was completed, the reaction solution was concentrated to dryness under reduced pressure. Purification by column chromatography yielded 2.1 g of the impurity compound of Urapidil (yield 18.9%, purity 94.0%).

[0053] Product characterization of urapidil impurity compound:

[0054] (1) Perform mass spectrometry analysis (ESI-MS) on the urapidil impurity compound prepared in Example 1: m / z=432.2[M+H]+, the mass spectrum of urapidil impurity compound is as follows figure 1 shown.

[0055] (2) NMR analysis of the urapidil impurity compound prepared in ...

Embodiment 2

[0058] The preparation method of urapidil impurity compound is as follows:

[0059] Add 10 g of urapidil, 20 mL of methanol, and 20 mL of water into the pressure reaction vessel, remove the air in the reaction vessel with carbon dioxide gas, pass the carbon dioxide gas to the set pressure of 40 psi, and keep the temperature at 50°C for 16 hours. After the reaction was completed, the reaction solution was concentrated to dryness under reduced pressure. Purified by column chromatography, the product of the impurity compound of urapidil was 1.8 g (yield 16.2%, purity 93.3%).

Embodiment 3

[0061] The preparation method of urapidil impurity compound is as follows:

[0062] Add 10 g of urapidil, 10 mL of acetone, and 20 mL of water into the pressure reaction vessel, remove the air in the reaction vessel with carbon dioxide gas, pass the carbon dioxide gas to the set pressure of 50 psi, and keep the temperature at 50°C for 16 hours. After the reaction was completed, the reaction solution was concentrated to dryness under reduced pressure. Purified by column chromatography to obtain 1.7 g of the impurity compound of urapidil (yield 15.3%, purity 92.1%).

[0063] The present invention characterizes the urapidil impurity compound prepared in Examples 2 and 3, and the result is consistent with the impurity characterization conclusion of Example 1.

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Abstract

The invention belongs to the technical field of medicine impurity preparation, and discloses an urapidil impurity compound, a preparation method and application thereof. The preparation method of theurapidil impurity compound comprises the following steps that 1), urapidil is dissolved in a mixed solvent of an organic solvent and water, and after heating dissolution is completed, carbon dioxide is introduced for a pressurization reaction; and 2) after the reaction is finished, the reaction solution isconcentrated and dried under reduced pressure, and purifying is carried out by column chromatography to obtain the urapidil impurity compound. The impurity compound meets the requirements of an impurity reference substance in quality control, can be used for quality control in a urapidil or urapidil hydrochloride synthesis process, can be used as the impurity reference substance for accurate quantitative detection of urapidil or urapidil hydrochloride, and is beneficial to improvement ofquality control of corresponding bulk drugs.

Description

technical field [0001] The invention relates to the technical field of pharmaceutical impurity preparation, in particular to an urapidil impurity compound, a preparation method and an application thereof. Background technique [0002] Urapidil (Urapidil), structural formula II is a highly selective α-receptor blocker with both peripheral and central effects. The peripheral vasodilation effect is mainly to block the post-synaptic α1 receptor, so that the peripheral resistance is significantly reduced, and the central effect is to reduce blood pressure by activating the 5-hydroxytryptamine-1A receptor and reducing the sympathetic feedback regulation of the medullary cardiovascular center. Urapidil preparations have two dosage forms: oral and injection. The raw material used in the oral dosage form is Urapidil, and the raw drug used in the injection is Urapidil Hydrochloride (Urapidil Hydrochloride), with a structural formula such as formula III. Urapidil sustained-release tab...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D239/545G01N30/02G01N30/06
CPCC07D239/545G01N30/02G01N30/06
Inventor 秦勇周超赵维王勇
Owner 燃点(南京)生物医药科技有限公司
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