A kind of preparation method of urapidil hydrochloride

A technology of uradil hydrochloride and uradil, which is applied in organic chemistry and other fields, and can solve the problems of large pollution, low yield, and high cost

Active Publication Date: 2021-07-02
HEBEI YIPIN PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The inventor has conducted research on the methods disclosed above, and found that the main disadvantages of these patents are: low yield, high pollution, high cost, and difficult operation in large-scale production

Method used

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  • A kind of preparation method of urapidil hydrochloride
  • A kind of preparation method of urapidil hydrochloride
  • A kind of preparation method of urapidil hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0032] The preparation of example 1 urapidil hydrochloride

[0033] A. Preparation of Urapidil

[0034] Add 3-[4-(2-methoxyphenyl)piperazin-1-yl]propylamine (50.00g, 0.20mol) and 6-chloro-1,3-dimethylurea to a 500ml clean three-necked reaction flask Pyrimidine purified water (35.01g, 0.20mol), sodium hydroxide (24.06g, 0.60mol) and purified water (500ml), mechanically stirred, heated to 60°C for 2 hours, cooled to room temperature, suction filtered, and the filter cake was ℃ blast drying for 6 hours to obtain 41.2 g of urapidil with a yield of 53.0% and a purity of 96.5%.

[0035] B. Preparation of Urapidil Hydrochloride

[0036] Add absolute ethanol (200.00g) and urapidil (20.00g, 0.05mol) to a 500ml clean three-necked reaction flask and heat up to 70-80°C, dropwise add a mixed solution of hydrochloric acid and ethanol solution (7.32g concentrated hydrochloric acid and 8.00g After the addition, keep stirring at 70-80°C for 1.0h, cool down to room temperature, filter with s...

example 2

[0037] The preparation of example 2 urapidil hydrochloride

[0038] A. Preparation of Urapidil

[0039] Add 3-[4-(2-methoxyphenyl)piperazin-1-yl]propylamine (50.00g, 0.20mol) and 6-chloro-1,3-dimethylurea to a 500ml clean three-necked reaction flask Pyrimidine purified water (35.01g, 0.20mol), potassium hydroxide (33.66g, 0.60mol) and purified water (500ml), stirred mechanically, heated to 60°C for 2 hours, cooled to room temperature, suction filtered, and the filter cake was ℃ blast drying for 6 hours to obtain 38.9 g of urapidil with a yield of 50.1% and a purity of 95.8%.

[0040] B. Preparation of Urapidil Hydrochloride

[0041] Add absolute ethanol (200.00g) and urapidil (20.00g, 0.05mol) to a 500ml clean three-necked reaction flask and heat up to 70-80°C, dropwise add a mixed solution of hydrochloric acid and ethanol solution (7.32g concentrated hydrochloric acid and 8.00g After the addition, keep stirring at 70-80°C for 1.0h, cool down to room temperature, filter wit...

example 3

[0043] Preparation of Urapidil Hydrochloride

[0044] A. Preparation of Urapidil

[0045] Add 3-[4-(2-methoxyphenyl)piperazin-1-yl]propylamine (50.00g, 0.20mol) and 6-chloro-1,3-dimethylurea to a 500ml clean three-necked reaction flask Pyrimidine purified water (35.01g, 0.20mol), anhydrous sodium carbonate (63.59g, 0.60mol) and purified water (500ml), stirred mechanically, heated to 60°C for 2 hours, cooled to room temperature, suction filtered, and the filter cake was 66.23 g of urapidil was obtained by blast drying at 50°C for 6 hours, with a yield of 85.2% and a purity of 97.9%.

[0046] B. Preparation of Urapidil Hydrochloride

[0047] Add dehydrated ethanol (400.00g) and urapidil (40.00g, 0.10mol) to a 500ml clean three-necked reaction flask and heat up to 70-80°C, add dropwise a mixed solution of hydrochloric acid and ethanol solution (14.64g concentrated hydrochloric acid and 16.00g After the addition, keep stirring at 70-80°C for 1.0h, cool down to room temperature,...

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Abstract

The present invention relates to a new preparation method of urapidil hydrochloride, which uses 3-[4-(2-methoxyphenyl) piperazin-1-yl] propylamine and 6-chloro-1,3- Urapidil is prepared from dimethyluracil as an intermediate, and then urapidil hydrochloride is obtained through salt formation. The new preparation process of urapidil hydrochloride according to the present invention has simple raw material structure, uses water as solvent, easy post-treatment, product purity, the total amount of related substances is less than 0.3%, and the yield is relatively high, the total yield is greater than 79%. , suitable for industrial production.

Description

Technical field: [0001] The invention relates to a preparation method of a pharmaceutical compound, in particular to a novel method for preparing urapidil hydrochloride. Background technique: [0002] Hypertension is one of the diseases that seriously threaten human health at present. It is the main cause of coronary heart disease, congestive heart failure and stroke. Among the causes of renal failure, hypertension is second only to diabetes. At present, the high blood pressure in clinical application should include adrenoceptor blockers, calcium antagonists, diuretics, etc. according to the mechanism of action. Among them, the new generation of α-receptor blockers represented by urapidil hydrochloride has been clinically recommended as the first-line antihypertensive drug because of its definite antihypertensive effect, less adverse reactions, and certain blood lipid-lowering effect. Research and development has good social and managerial benefits. [0003] The chemical n...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D239/545
CPCC07D239/545
Inventor 张辑陈文辉吕帅刘雪松段士宝李铭皓程瑶赵翠然张永然
Owner HEBEI YIPIN PHARMA
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