Method for synthesizing N,N-diethylamino ethanethiol

A technology of diethylaminoethanethiol and ethylaminoethanethiol, which is applied in the field of N, can solve the problems of high recovery energy consumption, low yield, poor product quality, etc., achieve environmental protection, high yield, and prevent self-polymerization Effect

Active Publication Date: 2009-07-15
河北远大九孚生物科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0020] In this method, N, N diethylaminoethanethiol is synthesized by pressurized reaction with ethylene thiolane and diethylamine, and needs to be reacted in an organic solvent. The amount of solvent used is large, and the recovery energy consumption is large, and it is difficult to avoid The alkane itself polymerizes into a white solid, which eventually leads to poor product quality and low yield

Method used

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  • Method for synthesizing N,N-diethylamino ethanethiol

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Embodiment 1

[0041] In a 500-liter reactor, 60 kilograms of ethylene sulfide were first added and stirred, then 180 kilograms of diethylamine were added, and 2 kilograms of petroleum ether were added, followed by stirring, and the temperature was refluxed at 60°C. After the reaction was completed for 10 hours, diethylamine and petroleum ether were recovered by distillation, and then 107 kg of N,N-diethylaminoethanethiol was obtained by distillation under reduced pressure.

[0042] The reaction equation of the present embodiment is:

[0043]

[0044] The mass percentage concentration of N,N-diethylaminoethanethiol in this embodiment is 99%, and the yield can reach 95.5%.

Embodiment 2

[0046] In a 2000-liter reactor, 240 kilograms of ethylene sulfide were first added and stirred, then 1200 kilograms of diethylamine were added, and 4 kilograms of sodium borohydride were added, followed by stirring and heating at 55°C. Reflux reaction for 15 hours, after the reaction is completed, diethylamine and sodium borohydride are recovered by distillation, and then 435 kg of N,N diethylaminoethanethiol can be obtained by distillation under reduced pressure.

[0047] The mass percentage concentration of N,N diethylaminoethanethiol in this embodiment is 99%, and the yield can reach 96.4%.

[0048] The reaction equation of the present embodiment is:

[0049]

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Abstract

The invention relates to a synthetic method for N, N-diethylaminoethanethiol, comprising the following step: the N, N-diethylaminoethanethiol is prepared after mixing ethylene sulfide and diethylamine under the condition of adding catalyst and heating the mixture to 50-80 DEG C for reaction. In the method, under the condition of presence of the catalyst, the raw materials can fully react without using any solvent and the ethylene sulfide can be effectively prevented from self polymerization, thus obtaining the products with high yield and quality. Meanwhile, without producing the three wastes, the method effectively protects the environment.

Description

technical field [0001] The invention relates to a method for synthesizing a compound, in particular to a method for synthesizing N,N diethylaminoethanethiol. Background technique [0002] N, N diethylaminoethane mercaptan is a key intermediate in the production of veterinary fungicide tiamulin. Due to the gradual expansion of domestic and foreign markets for tiamulin in recent years, the intermediate N, N diethylamino ethanethiol has The demand has also increased, about 250 tons / year. According to the records of domestic and foreign documents, there are altogether six process routes in the prior art, which are respectively ethyl chloroformate route, thiohydrogen salt route, thiocyanate route, benzyl mercaptan route, thiourea route and ethylene sulfide route. [0003] Wherein, the ethyl chloroformate route is as follows: [0004] [0005] This method has a long route and uses hydroxyethane mercaptan, a highly toxic controlled product, so it is not easy to obtain and th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C323/25C07C319/06B01J31/02B01J31/14
CPCY02P20/584
Inventor 赵云现李超
Owner 河北远大九孚生物科技有限公司
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