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Preparation method for trifluoroethylamine hydrochloride

A technology of trifluoroethylamine hydrochloride and trifluoroethylamine, applied in the field of preparation of trifluoroethylamine hydrochloride, can solve the problem that the solvent ether is flammable, the neutralizing agent hydrogen chloride gas is not easy to obtain and use, and it is not easy to industrialize application, etc.

Active Publication Date: 2016-07-27
ZHEJIANG LANTIAN ENVIRONMENTAL PROTECTION HI TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The solvent diethyl ether used in this method is flammable, and the neutralizing agent hydrogen chloride gas is difficult to obtain and use, and is not easy for industrial application

Method used

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  • Preparation method for trifluoroethylamine hydrochloride
  • Preparation method for trifluoroethylamine hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Add 100g of ethanol and 33g of trifluoroethylamine into the three-necked flask, slowly add 35g of saturated hydrochloric acid solution dropwise when the temperature is lower than 25°C, and keep the temperature for one hour for reaction after the dropwise addition is completed. The reaction solution after the reaction was subjected to vacuum distillation and desolventization operation, the vacuum degree of the control system was 0.080MPa, and the temperature was 50±5°C. After 5 hours of vacuum distillation and desolventization operation, the water and ethanol were completely removed to obtain three Fluoroethylamine hydrochloride 40.8g, product yield is 90.33%. The obtained trifluoroethylamine hydrochloride is a white powdery crystalline solid with a water content of 0.15% (the water content of the product is measured with a Karl Fischer moisture meter, the same below).

Embodiment 2

[0017] Add 100g of ethanol and 33g of trifluoroethylamine into the three-neck flask, slowly add 35g of saturated hydrochloric acid solution dropwise when the temperature is lower than 25°C, and then raise the temperature to 50°C and keep it warm for one hour. After the reaction, the vacuum degree of the reaction solution in the system is 0.098MPa, the temperature is controlled at 45±5°C, and the water and ethanol are removed after 5 hours of vacuum distillation and desolvation operation to obtain trifluoroethylamine hydrochloride 43.5 g, the product yield is 96.30%. The obtained trifluoroethylamine hydrochloride is a white powdery crystalline solid with a water content of 0.13%.

Embodiment 3

[0019] Add 100g of ethanol and 33g of trifluoroethylamine into the three-neck flask, slowly add 35g of saturated hydrochloric acid solution dropwise when the temperature is lower than 25°C, and then raise the temperature to 50°C and keep it warm for one hour. After the reaction, the vacuum of the reaction solution in the system is 0.070MPa, the temperature is controlled at 55±5°C, and the water and ethanol are removed after 5 hours of vacuum distillation and desolventization to obtain trifluoroethylamine hydrochloride 41.8g, the product yield is 92.54%. The obtained trifluoroethylamine hydrochloride is a white powdery crystalline solid with a water content of 0.23%.

[0020] Table 1

[0021]

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Abstract

The invention discloses a preparation method for trifluoroethylamine hydrochloride. The preparation method comprises the following steps: subjecting trifluoroethylamine and hydrochloric acid to neutralization reaction in an ethanol-water azeotropic or near-azeotropic system so as to obtain a trifluoroethylamine hydrochloride contained solution after reaction, and removing water and ethanol through reduced pressure distillation and desolvation so as to obtain trifluoroethylamine hydrochloride. The method provided by the invention has safe process, and prepared trifluoroethylamine hydrochloride has high purity and low water content.

Description

technical field [0001] The invention relates to a preparation method of trifluoroethylamine hydrochloride. Background technique [0002] Trifluoroethylamine hydrochloride, pale yellow or white crystal in appearance, English name trifluoroethylaminehydrochloride, CAS No. 373-88-6, molecular weight 135.5, molecular formula C 2 h 4 f 3 N·HCl, melting point 220-222°C, insoluble in ether, good solubility in absolute ethanol, easily soluble in water. [0003] Trifluoroethylamine hydrochloride is a widely used fluorine-containing organic compound. In the field of medicine, drug intermediates and finished drugs synthesized from it can be used to treat various cardiovascular diseases, mental diseases, bacterial or viral infections , cancer, immune regulation disorder, malaria, stomach disease, etc. In the field of agriculture, trifluoroethylamine hydrochloride is used to synthesize a variety of pesticides. Trifluoroethylamine hydrochloride can also be used as a synthetic veterin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/15C07C209/00
Inventor 徐卫国李华陈伟蒋强
Owner ZHEJIANG LANTIAN ENVIRONMENTAL PROTECTION HI TECH
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