Preparation method of tetraimidazole free alkali

A technology of free base and tetramisole, which is applied in the field of preparation of tetramisole free base, can solve the problems of long reaction steps, uneconomical, cost increase, etc.

Active Publication Date: 2020-07-07
SHANDONG GUOBANG PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But it also went through a long reaction step
Moreover, the introduction of organic solvents brings about cost increases and environmental protection issues, which is not economical enough

Method used

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  • Preparation method of tetraimidazole free alkali
  • Preparation method of tetraimidazole free alkali
  • Preparation method of tetraimidazole free alkali

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Using a 2L four-neck flask, add 1000 g of a buffer solution of ammonium chloride and ammonia water, and raise the temperature to 60°C. At a speed of 500-600rpm, using a micro-quantitative feeder, a total of 200g of N-(2-chloroethyl)-α-(chloromethyl)-benzylamine hydrochloride solid and a total of 71.67g of Thiourea solid (molar ratio 1:1.2), where the feeding rate of N-(2-chloroethyl)-α-(chloromethyl)-benzylamine hydrochloride is 1.11g / min, the feeding speed of thiourea It is 0.4g / min, and the dosing is completed in 3h. During the reaction, the pH of the solution will decrease continuously. Use 30% sodium hydroxide solution to control the pH value, so that the pH value of the reaction solution is controlled at pH=9. After feeding is complete, heat up to 80~85°C, keep warm for 2.5h, cool down to 25°C, obtain 148.75g product after filtration, detect purity 98.56%, calculate and obtain the yield of tetramisole free base 91.45%.

Embodiment 2

[0036] Similar to Example 1, wherein the initial reaction temperature was adjusted to 55°C. Finally, 144.64 g of the product was obtained by filtration, the detection purity was 98.83%, and the calculated yield was 89.17%.

Embodiment 3

[0038] Similar to Example 1, wherein the initial reaction temperature was adjusted to 65°C. Finally, 141.08 g of the product was obtained by filtration, the detection purity was 96.87%, and the calculated yield was 85.25%.

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Abstract

The invention discloses a preparation method of tetraimidazole free alkali. Alpha-[[(2-hydroxyethyl)amino]methyl]benzyl alcohol reacts with thionyl chloride, then water is added for heating dissolution, after activated carbon thermal filtration, N-(2-chloroethyl)-alpha-(chloromethyl)-benzylamine hydrochloride is obtained through cooling crystallization, then N-(2-chloroethyl)-alpha-(chloromethyl)-benzylamine hydrochloride and thiourea are subjected to direct cyclization, and tetraimidazole free alkali is generated. The method is simple in production process, mild in reaction condition and highin total yield, the production cost is reduced, the generation amount of three wastes is small, the double contradiction between economy and environment in the development process of modern enterprises is well solved, and the production process has great competitiveness and good industrial prospects.

Description

technical field [0001] The invention belongs to the technical field of pharmaceutical production, in particular to a method for preparing tetramisole free base. Background technique [0002] Tetramisole free base is an intermediate for the preparation of tetramisole hydrochloride. Tetramisole hydrochloride, also known as thimidazole hydrochloride, tetramisole, Quchongjing, etc., chemical name DL-2,3,5,6-tetrahydro-6-phenylimidazo[2,1-b]thiazole hydrochloride, Molecular formula C 11 h 12 N 2 S·HCl, relative molecular weight 240.75, CAS No. 5086-74-8. White crystalline powder, odorless, bitter and astringent. Soluble in water and methanol, slightly soluble in ethanol, very slightly soluble in chloroform, insoluble in acetone. Tetramisole hydrochloride is a high-efficiency broad-spectrum drug anthelmintic, which has good curative effect on infections such as roundworms, hookworms, and pinworms. Its structural formula is: [0003] [0004] Tetramisole is the precursor ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D513/04
CPCC07D513/04
Inventor 程贺刘聪乔建超王友杰
Owner SHANDONG GUOBANG PHARMA
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