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A kind of preparation method of diethylaminoethanethiol

A kind of technology of diethylaminoethane mercaptan and diethylamino halogenated hydrocarbon is applied in the field of preparation of diethylaminoethane mercaptan obtained by reduction, can solve problems such as few reports of diethylamino ethane mercaptan, and achieves low cost and high yield. High efficiency and simple operation

Active Publication Date: 2018-12-28
保定加合精细化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] According to references at home and abroad, it is found that there are fewer reports about diethylaminoethanethiol

Method used

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  • A kind of preparation method of diethylaminoethanethiol
  • A kind of preparation method of diethylaminoethanethiol
  • A kind of preparation method of diethylaminoethanethiol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Add 120mL of ethanol and 30mL of water into a 500mL three-necked bottle, then add 24.49g of sodium disulfide, stir for 1.5h, slowly add 40.97g of diethylaminochloroethane dropwise, after the addition, react at reflux temperature to control the reaction The temperature was 15°C, stirred for 8h, followed by TLC until the end of the reaction. Extract with toluene, separate the phases, and concentrate the organic phase to obtain 37.87 g of disulfide. GC-MS detection, the spectrum is as figure 2 , compared with the standard sample, the spectrum Figure 1 Sincerely.

[0027] (2) Add 36.67g of disulfide to a 500mL three-necked flask, add the reducing agent Fe / HCl, add 11.67g of iron, slowly add 76.06g of 20% HCl, keep the temperature at 20°C, stir for 10h, and the reaction ends. Sampling was performed by HPLC for quantification, and 48.78 g of diethylaminoethanethiol was obtained, with a conversion rate of 96.3%. GC-MS detection, the spectrum is as figure 1 , compare...

Embodiment 2

[0030] (1) Add 120mL of ethanol and 40mL of water into a 500mL three-necked bottle, then add 26.94g of sodium disulfide, stir for 1.5h, slowly add 44.25g of diethylaminochloroethane dropwise, after the addition, react at reflux temperature to control the reaction The temperature was 15°C, stirred for 10 h, followed by TLC until the reaction was completed. Extract with toluene, separate the phases, and concentrate the organic phase to obtain 40.90 g of disulfide.

[0031] (2) Add 40.12g of disulfide to a 500mL three-necked flask, add the reducing agent Fe / HCl, add 8.51g of iron, slowly add 83.16g of 20% HCl, keep the temperature at 20°C, stir for 10h, and the reaction ends. Sampling was performed by HPLC for quantification, and 38.98 g of diethylaminoethanethiol was obtained, with a conversion rate of 96.3%.

[0032] HPLC method: detector: evaporative laser scattering detector; mobile phase: 5mmol•L-1 sodium dihydrogen phosphate-methanol (90:10); injection volume: 20uL.

Embodiment 3

[0034] (1) Add 120mL of ethanol and 60mL of water into a 500mL three-necked bottle, then add 30.94g of sodium disulfide, stir for 1.5h, slowly add 50.88g of diethylaminochloroethane dropwise, after the addition, react at reflux temperature to control the reaction The temperature was 15°C, stirred for 12 hours, followed by TLC until the reaction was completed. Extract with toluene, separate the phases, and concentrate the organic phase to obtain 47.03 g of disulfide.

[0035] (2) Add 46.89g of disulfide to a 500mL three-necked flask, add the reducing agent Fe / HCl, add 19.89g of iron, slowly add 20% HCl 324.14g, keep the temperature at 20°C, stir for 10h, and the reaction ends. Sampling was performed by HPLC for quantification, and 45.55 g of diethylaminoethanethiol was obtained, with a conversion rate of 96.3%. The mass spectrogram is consistent with the standard sample.

[0036] HPLC method: detector: evaporative laser scattering detector; mobile phase: 5mmol·L-1 sodium dihy...

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Abstract

The invention relates to a preparation method of diethylaminoethyl mercaptide. The preparation method comprises the following steps of (1) adding an organic solvent and water into a mixing container; then, adding sodium disulfide, stirring for 1 to 2h, slowly dripping lignocaine halogenated hydrocarbon, controlling the reaction temperature to 15 to 20 DEG C until the reaction is finished, and generating disulfide; (2) adding the disulfide obtained in step (1) into the other container, slowly adding a reducing agent, maintaining temperature to 20 DEG C, stirring for 8 to 12h until the reaction is finished, and generating the diethylaminoethyl mercaptide. The preparation method has the advantages that the operation is simple, the cost is low, and the yield rate is high.

Description

technical field [0001] The invention relates to a method for preparing diethylaminoethanethiol, in particular to a method for preparing diethylaminoethanethiol by taking diethylaminohalogenated hydrocarbon and sodium disulfide as raw materials and then reducing them. Background technique [0002] Tiamulin is a special diterpene antibiotic for livestock and poultry, which is used to prevent and treat poultry respiratory diseases and promote animal growth. Diethylaminoethanethiol is an important intermediate in the production of tiamulin. [0003] 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 following several methods for preparing diethylaminoethanethiol at present: monosulfate and sodium hydrosulfide method; (2) diethylaminochloroethane and sodium hydrosulfide method; (3) monosulfuric acid Vinegar and thiourea method: (4) thioether method. [0004]...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C319/06C07C323/25
CPCC07C319/06C07C319/22C07C323/25
Inventor 孙凤霞李姝靓王玉春韩珊王静云
Owner 保定加合精细化工有限公司