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Preparation method of trifluoroethylamine

A technology of trifluoroethylamine and difluoroethylamine, which is applied in the field of preparation of trifluoroethylamine, can solve problems such as difficult industrialization, numerous routes, and difficult operation, and achieve low cost, easy cost, and simple reaction operation Effect

Inactive Publication Date: 2016-08-31
NANTONG BAOKAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the raw material cost of this route is relatively cheap, there are many routes, difficult operation and low yield, and it is also difficult to industrialize

Method used

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  • Preparation method of trifluoroethylamine

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Such as figure 1 Shown, a kind of preparation method of trifluoroethylamine comprises the steps:

[0025] The first step, amination reaction: with CHF 2 CH 2 X is a raw material, and in the presence of a solvent and a catalyst, it is ammoniated with ammonia gas to generate trifluoroethylamine, and the reaction equation is as follows:

[0026] CHF 2 CH 2 Cl + 2NH 3 → CF 3 CH 2 NH 2 +NH 4 Cl;

[0027] The solvent is: NMP or DMF.

[0028] The specific operation of the amination reaction is as follows: using a batch process, add solvent, liquid ammonia and an appropriate amount of catalyst in sequence in a high-pressure reactor equipped with an exhaust gas absorption device, start stirring, heat up, and slowly feed CHF at a specified speed at 30°C 2 CH 2 Cl reaction, observe the internal temperature of the kettle. When the temperature of the kettle rises to about 110°C, the pressure of the kettle is at 2.0MPa, and the reaction is kept for 16 hours. The reactio...

Embodiment 2

[0032] Such as figure 1 Shown, a kind of preparation method of trifluoroethylamine comprises the steps:

[0033] The first step, amination reaction: with CHF 2 CH 2 Br is a raw material, and in the presence of a solvent and a catalyst, ammonia gas is ammoniated to generate trifluoroethylamine, and the reaction equation is as follows:

[0034] CHF 2 CH 2 Br + 2NH 3 → CF 3 CH 2 NH 2 +NH 4 Br;

[0035] The solvent is: DMSO.

[0036] The specific operation of the amination reaction is as follows: using a batch process, add solvent, liquid ammonia and an appropriate amount of catalyst in sequence into a high-pressure reactor equipped with an exhaust gas absorption device, start stirring, heat up, and slowly feed CHF at a specified speed at 100°C 2 CH 2 Br reaction, observe the internal temperature of the kettle. When the temperature of the kettle rises to about 210°C, the pressure of the kettle is at 6.0MPa, and the reaction is kept for 36 hours. The reaction is basic...

Embodiment 3

[0040] Such as figure 1 Shown, a kind of preparation method of trifluoroethylamine comprises the steps:

[0041] The first step, amination reaction: with CHF 2 CH 2 I is a raw material, and in the presence of a solvent and a catalyzer, ammonia gas is ammoniated to generate trifluoroethylamine, and the reaction equation is as follows:

[0042] CHF 2 CH 2 I + 2NH 3 → CF 3 CH 2 NH 2 +NH 4 I;

[0043] The solvent is: alkyl glycol: propylene glycol or ethylene glycol.

[0044] The specific operation of the amination reaction is as follows: using a batch process, add solvent, liquid ammonia and an appropriate amount of catalyst sequentially into a high-pressure reactor equipped with an exhaust gas absorption device, start stirring, heat up, and slowly feed CHF at a specified speed at 80°C 2 CH 2 1 reaction, observe the temperature situation in the kettle, when the temperature of the kettle rises to about 170°C, the pressure of the kettle is at 4.0MPa, and the heat pres...

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Abstract

The invention discloses a preparation method of trifluoroethylamine. The preparation method comprises the following steps: amination reaction: taking CHF2CH2X as a raw material, and feeding ammonia gas in the presence of a solvent and a catalyst to ammonify so as to generate trifluoroethylamine; and rectification: rectifying the ammonified product to obtain a finished product, filtering kettle liquid to obtain ammonium chloride as a by-product, and recycling filtrate used as the solvent of amination reaction. The catalyst is inorganic iodide, and the solvent is a frequently used organic solvent DMF or NMP. The purity of the prepared finished product is greater than or equal to 99.5%, and the yield of the finished product is greater than or equal to 90%.

Description

technical field [0001] The invention belongs to the field of organic intermediates, in particular to a preparation method of trifluoroethylamine. Background technique [0002] Trifluoroethylamine is an important organic intermediate widely used in pesticide, pharmaceutical and chemical industries. In the field of pesticides, highly active insecticides, acaricides, ovicides, and herbicides can be synthesized. In the field of medicine, it can be used as a medicine intermediate to prepare 1,2-substituted biguanide and its derivatives for treating diabetes. [0003] Its synthesis mainly has the following routes: [0004] In 1934, Henry Gilman used sodium trifluoroacetate as a raw material to generate trifluoroacetonitrile through esterification, amidation, and dehydration of phosphine pentoxide, and finally obtained the target product trifluoroethylamine by platinum-catalyzed hydrogenation. This route step is longer, and operation is complicated, and total yield is lower, has...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/15C07C209/08C07C209/84
CPCC07C209/08C07C209/84C07C211/15
Inventor 闫宗刚张林林黄凯华周佳欢
Owner NANTONG BAOKAI CHEM
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