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Synthesis process of diethylaminoethanethiol

A technique for the synthesis of diethylaminoethanethiol, which is applied in the fields of mercaptan preparation and organic chemistry, and can solve problems such as harsh reaction conditions, environmental pollution, and low product purity, and achieve the effect of reducing side reactions

Pending Publication Date: 2021-09-14
新疆上昵生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The above-mentioned processes have problems such as harsh reaction conditions, environmental pollution, or low product purity.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] For the addition reaction of diethylamine and ethylene sulfide, vacuumize the closed addition kettle, the vacuum degree is -0.097 MPa, fill it with nitrogen, repeat 1-2 times, and press the diethylamine into the addition reaction through the meter with nitrogen. In the kettle, continue to fill nitrogen to the micro-pressure level of 0-0.3 kpa, start the stirring, the stirring speed is 100-120 r / min, and when the temperature rises to 58°C, start to slowly feed ethylene sulfide at constant pressure, and the feeding time For 2 hours, the feeding amount is based on the molar ratio of sulfide to diethylamine 1:1.51. After the addition of sulfide is completed, the reaction is continued for 6 hours, and the addition tank maintains weakly alkaline conditions. While reacting, continuously feed nitrogen into the reactor to maintain a slight pressure of 0-0.3 kpa. Exhaust gas enters the RTO system for combustion to ensure compliance with emission standards.

[0025] Distillation,...

Embodiment 2

[0027] Addition reaction of diethylamine and ethylene sulfide, add its mass fraction 6% sodium hydroxide catalyst, and heat up to 56°C, start to slowly add sulfide at constant pressure, and the flow rate is based on ethane sulfide With diethylamine mol ratio 1:2, other are with embodiment 1.

[0028] Distillation, normal pressure distillation reclaims excess 279.83 kg diethylamine to the storage tank, vacuum distillation receives 550.85 kg diethylaminoethanethiol to the storage tank, the reaction yield is 96.7%, and the others are the same as in Example 1.

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PUM

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Abstract

A synthesis process of diethylaminoethanethiol comprises the following steps: carrying out an addition reaction on ethylene sulfide synthesized by sodium thiocyanate and ethylene carbonate and excessive diethylamine in an addition kettle, distilling the reaction product in a distillation kettle, carrying out atmospheric distillation to collect unreacted diethylamine, directly recycling the unreacted diethylamine, carrying out reduced pressure distillation on the reaction product, and removing impurities to obtain the diethylaminoethanethiol. The preparation method of diethylaminoethanethiol is reasonable in process, green and environment-friendly, and high in product purity.

Description

technical field [0001] The invention relates to the technical field of pharmaceutical intermediate manufacture, in particular to a synthesis process of diethylaminoethanethiol. Background technique [0002] The chemical name of 2-Diethylaminoethanethiol (2-Diethylaminoethanethiol) is 2-Diethylaminoethanethiol, and its molecular formula is C 6 h 15 NS, it is an important raw material for the preparation of veterinary antibiotic Tiamulin fumarate. In recent years, due to the rapid development of the centralized breeding industry, the demand for tiamulin fumarate has been rising steadily, so the demand for diethylaminoethanethiol, the key raw material of tiamulin fumarate, has also increased in pharmaceutical companies. increase. [0003] At present, the industry generally adopts the addition reaction of ethylene sulfide and diethylamine to prepare diethylaminoethanethiol. Since sulfide will accelerate self-polymerization in the presence of water, how to dehydrate raw mater...

Claims

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Application Information

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IPC IPC(8): C07C323/25C07C319/06
CPCC07C319/06C07C323/25
Inventor 陈剑慧陈鑫亮沈敏祥朱菊芬张丽学
Owner 新疆上昵生物科技有限公司
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