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Process for synthesizing diethylaminoethyl mercaptide

A technology of diethylaminoethanethiol and synthesis process, applied in the direction of mercaptan preparation, organic chemistry, etc., can solve the problem of high cost and achieve the effect of high product yield and purity

Inactive Publication Date: 2014-05-28
张丽学
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method needs to be carried out under pressurized conditions, which has certain safety hazards and high cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Add 560 grams of potassium thiocyanate into a 2000ml four-necked flask (equipped with a temperature-adjusting heater, a thermometer at 50-250°C, connected to a 400mm spherical condenser and a receiving bottle, connected to a vacuum pump, and connected to circulating water on the condenser), and open The power supply of the heating mantle starts to heat up slowly. When the temperature in the bottle rises to 120°C, turn on the vacuum pump to evacuate (vacuum degree -0.085MPa), and the material in the bottle gradually begins to melt. At this time, the material is completely melted, and there are many boiling bubbles. After there are no bubbles, stop heating, stop the vacuum pump, and naturally cool down to 50-60 ° C. The material in the bottle is solid, showing light blue-gray.

[0017] Melt ethylene carbonate in advance, weigh 500g, and add it to the four-necked flask in the above steps (the bottle is equipped with a 50-200°C thermometer, connected to a 600mm condenser, pa...

Embodiment 2

[0021] Add 560 grams of potassium thiocyanate into a 2000ml four-necked flask (equipped with a temperature-adjusting heater, a thermometer at 50-250°C, connected to a 400mm spherical condenser and a receiving bottle, connected to a vacuum pump, and connected to circulating water on the condenser), and open The power supply of the heating mantle starts to heat up slowly. When the temperature in the bottle rises to 120°C, turn on the vacuum pump to evacuate (vacuum degree -0.085MPa), and the material in the bottle gradually begins to melt. At this time, the material is completely melted, and there are many boiling bubbles. After there are no bubbles, stop heating, stop the vacuum pump, and naturally cool down to 50-60 ° C. The material in the bottle is solid, showing light blue-gray.

[0022] Melt ethylene carbonate in advance, weigh 500g, and add it to the four-necked flask in the above steps (the bottle is equipped with a 50-200°C thermometer, connected to a 600mm condenser, pa...

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PUM

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Abstract

The invention discloses a process for synthesizing diethylaminoethyl mercaptide. The process comprises the following steps: pretreating raw materials, preparing thiirane through the reaction of potassium sulfocyanide and ethylene carbonate, and finally synthesizing the thiirane and diethylamine into the product of diethylaminoethyl mercaptide. In the synthesis process, pretreatment is firstly carried out on the raw materials, a sectional heating mode is adopted during synthesis reaction so as to enable the reactants to be reacted completely, no solvents or catalysts are added in the whole process, pressurizing is not required, the yield and purity of the product are high, three wastes are not generated, and the process is environment-friendly.

Description

technical field [0001] The invention belongs to the field of compound synthesis, in particular to a synthesis process of diethylaminoethanethiol. Background technique [0002] Tiamulin is a special diterpene antibiotic for livestock and poultry, which is used to prevent and treat respiratory diseases and promote animal growth. Diethylaminoethanethiol is an important intermediate in the production of tiamulin. [0003] Chinese patent 200810088884.5 discloses a preparation method of diethylaminoethanethiol, first diethylaminoethanol is chlorinated with a chlorinating agent to generate diethylaminochloroethane or its hydrochloride, and then diethylaminochloride Ethane or its hydrochloride reacts with thiourea to generate S-substituted isothiouronium salt, and finally the S-substituted isothiouronium salt is subjected to alkaline hydrolysis with a strong base to prepare diethylaminoethanethiol. The process of this method is relatively complicated, and water, alkali and other s...

Claims

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Application Information

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IPC IPC(8): C07C323/25C07C319/02
Inventor 张丽学
Owner 张丽学
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