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Method for preparing N, N-diethylamino ethanethiol

A technology for diethylaminoethane mercaptan and diethylamine, which is applied in the field of chemistry, can solve the problems of long synthesis process, many kinds of raw materials, difficult sources, etc., and achieves the effects of short process flow, few kinds of raw materials, and wide sources.

Inactive Publication Date: 2009-11-25
赵云现
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The product N,N-diethylaminoethanethiol is obtained by displacement reaction between diethylaminoethyl chloride and mercapto compound, but there are many problems such as long synthesis process, many wastes, many kinds of raw materials and difficult sources.

Method used

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  • Method for preparing N, N-diethylamino ethanethiol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Step a: Add 1 mole of potassium thiocyanate and 1 mole of ethylene carbonate into the reaction flask, heat up to 100°C under normal pressure, keep it warm for 7 hours, and distill out the boiling point of 54°C to 56°C after the reaction is completed. The distillate was 49 g of sulfide, and the content of the product was 99.7% according to gas chromatography analysis, and the yield was 81.4%.

[0029] Step b: Add 1 mole of sulfide, 1 mole of diethylamine and 200ml of toluene into the reaction flask, heat up to 50°C under normal pressure for reflux reaction, keep reflux for 15 hours, and distill out the boiling point after the reaction is completed The fraction at 160°C to 162°C is 127.6g of the product N,N-diethylaminoethanethiol, the content of the product is 99.5% and the yield is 95.5% through gas chromatography analysis.

Embodiment 2

[0031] Step a: Add 1 mole of potassium thiocyanate and 5 moles of ethylene carbonate into the reaction flask, heat it up to 130°C under normal pressure, and keep it warm for 10 hours. The distillate was 48.5 g of sulfide, and the content of the product analyzed by gas chromatography was 99.6%, and the yield was 80.5%.

[0032] Step b: Add 1 mole of sulfide, 1.8 moles of diethylamine and 200ml of toluene into the reaction flask, heat up to 60°C under normal pressure for reflux reaction, keep reflux for 21 hours, and distill out the boiling point after the reaction is completed The fraction at 160° C. to 162° C. is 127.9 g of the product N,N-diethylaminoethanethiol. The content of the product is 99.6% and the yield is 95.8% according to gas chromatography analysis.

Embodiment 3

[0034] Step a: Add 1 mole of potassium thiocyanate and 3 moles of ethylene carbonate into the reaction flask, heat it up to 150°C under normal pressure, keep it warm for 5 hours, and distill out the boiling point of 54°C to 56°C after the reaction is completed. The distillate was 49 g of sulfide, and the content of the product was 99.7% according to gas chromatography analysis, and the yield was 81.4%.

[0035] Step b: Add 1 mole of sulfide, 3 moles of diethylamine and 200ml of toluene into the reaction flask, heat up to 80°C under normal pressure for reflux reaction, keep reflux for 25 hours, and distill out the boiling point after the reaction is completed The fraction at 160°C to 162°C is 127.6g of the product N,N-diethylaminoethanethiol, the content of the product is 99.5% and the yield is 95.5% through gas chromatography analysis.

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Abstract

The present invention relates to a method for preparing N, N-diethylamino ethanethiol, belonging to a chemical technical field. The method includes steps of a. heating rhodanides and ethylene carbonate to react under ordinary pressure, distilling to obtain Thiirane after the reaction, the general formula of the rhodanides is M-SCN, wherein M is alkali metal of Na or K; b. mixing and stirring the Thiirane and diethylamine in a toluene dissolvant, heating under an ordinary pressure to implement a backflow reaction and distilling to obtain the N, N-diethylamino ethanethiol after the backflow reaction. The method has a short synthesis technical process, the kind of the raw materials is few and source is wide, the used toluene dissolvant may be recovered, and there will generate little waste water, waste gas and waste which may reduce environmental pollution.

Description

technical field [0001] The invention relates to a preparation method of a pharmaceutical intermediate, in particular to a preparation method of N,N-diethylaminoethanethiol, which belongs to the field of chemical technology. Background technique [0002] N,N-Diethylaminoethanethiol is an important raw material for pharmaceutical intermediates. It plays an increasingly important role in the production of pesticides and pharmaceuticals. With the wide application of this product, the international demand for this product is increasing year by year. [0003] There are many process routes for producing this product. At present, diethylamine is commonly used to react with ethylene oxide to obtain diethylaminoethanol, and then react with thionyl chloride to obtain diethylaminoethyl chloride. The product N,N-diethylaminoethanethiol is obtained by the displacement reaction between diethylaminoethyl chloride and mercapto compound, but there are long synthetic process flow, many wastes,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C323/25C07C319/06
Inventor 赵云现李超
Owner 赵云现
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