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A kind of preparation method of diethylaminoethanethiol

A technology for diethylaminoethanethiol and ethylaminoethanethiol is applied in the field of preparing diethylaminoethanethiol, which can solve the problems of difficult recovery of petroleum ether, high equipment cost, high price, etc. The effect of production energy consumption and production cost reduction

Active Publication Date: 2017-03-22
宁夏泰瑞制药股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The catalyzer that this method adopts is sherwood oil or sodium borohydride, and its existing problem is: 1, catalyzer sherwood oil is flammable, explosive, brings certain danger for large-scale process production, and sherwood oil is difficult to recover, pollutes environment; 2. Sodium borohydride is relatively safe, but it is difficult to recycle, the price is relatively expensive, and the production cost is high, so it is not suitable for mass industrial production
Due to the low boiling point of ethylene sulfide, it is dangerous to use a high-pressure reactor in this method, which is not suitable for large-scale production, and the equipment cost is high, so it does not have market competitiveness.

Method used

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  • A kind of preparation method of diethylaminoethanethiol

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 10kg of ethylene sulfide into a 100L closed reactor, stir slowly, then add 15kg of diethylamine, and after heating to 30°C, add 1kg of sodium hydroxide solution with a mass volume concentration of 2% dropwise. After the dropwise addition, the reaction 4 hours. After the reaction is completed, diethylamine is recovered by distillation, and then vacuum distillation is carried out to obtain diethylaminoethanethiol. The product yield is 98%, and the purity is 99%. Product purity was detected by gas chromatography.

Embodiment 2

[0021] Add 10kg of sulfide into a 100L closed reactor, stir slowly, then add 12kg of diethylamine, after heating to 35°C, add dropwise 1.1kg of sodium hydroxide solution with a mass volume concentration of 2.3%, and after the dropwise addition, React for 5 hours. After the reaction is completed, diethylamine is recovered by distillation, and then vacuum distillation is carried out to obtain diethylaminoethanethiol. The product yield is 97.6%, and the purity is 99.8%. Product purity was detected by gas chromatography.

Embodiment 3

[0023] Add 12kg of ethylene sulfide into a 100L closed reactor, stir slowly, then add 17kg of diethylamine, after heating to 40°C, add dropwise 1kg of sodium hydroxide solution with a mass volume concentration of 2.5%, after the dropwise addition, the reaction 5 hours. After the reaction is completed, diethylamine is recovered by distillation, and then vacuum distillation is carried out to obtain diethylaminoethanethiol. The product yield is 99%, and the purity is 98.9%. Product purity was detected by gas chromatography.

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Abstract

The invention relates to a preparation method for diethylaminoethanethiol. The preparation method comprises firstly putting ethylene sulfide in a sealed reactor, slowly stirring, adding ethene diamine, heating to 30 DEG C-40 DEG C, dropwise adding a sodium hydroxide solution, reacting for 4-5 h, distilling for recovering diethylamine, and finally performing reduced-pressure distillation to obtain diethylaminoethanethiol. According to the method, operation is simple, production is easy to realized, yield is relatively high, conditions are mild, addition of organic solvents and usage of a high-pressure reaction vessel are reduced, environment pollution and production cost are reduced.

Description

technical field [0001] The invention relates to a method for preparing diethylaminoethanethiol, in particular to a method for preparing diethylaminoethanethiol from ethylene sulfide and diethylamine as raw materials. Background technique [0002] Diethylaminoethanethiol (diethylaminoethanethiol) is a key intermediate in the production of veterinary drug tiamulin, and is in great demand in pharmaceutical companies. According to references at home and abroad, it is found that there are fewer reports about diethylaminoethanethiol. Wang Yanlin etc. mentioned in the patent that there are several methods for preparing diethylaminoethanethiol at present: (1) sulfuric acid monoester and sodium hydrosulfide method; (2) diethylaminochloroethane and sodium hydrosulfide method; (3) ) sulfuric acid monoester and thiourea method: (4) sulfide method. Because there are some defects in the above several methods, diethylaminoethanethiol is currently prepared in China using sulfide and dieth...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C319/06C07C323/25
Inventor 王义周丽娜王文超
Owner 宁夏泰瑞制药股份有限公司