Preparation method of 2,2-difluoroethylamine

A technology of difluoroethylamine and difluoroethanol, which is applied in the preparation of organic compounds, preparation of amino compounds, chemical instruments and methods, etc., which can solve the difficulty of continuous production in kettle reactions, difficulty in recycling catalysts, and difficulties in industrial production, etc. problems, to achieve the effects of easy continuous production, high reaction conversion rate and yield, and mild reaction conditions

Active Publication Date: 2014-09-10
HUBEI HAIZHIJIE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The technology disclosed in the above patents has some obvious defects, such as high temperature and high pressure, low yield, continuous production is not easy to achieve in kettle reaction, and it is difficult to recycle and apply expensive catalysts. Therefore, industrial production has certain difficulties

Method used

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  • Preparation method of 2,2-difluoroethylamine
  • Preparation method of 2,2-difluoroethylamine
  • Preparation method of 2,2-difluoroethylamine

Examples

Experimental program
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Effect test

Embodiment 1

[0030] In a single-tube reactor with a diameter of 20 mm, add 200 ml of alumina as a catalyst carrier, and under the conditions of a pressure of 0.5 MPa and a temperature of 180 ° C, and a hydrogen atmosphere, 2,2-difluoroethanol and liquid ammonia are introduced. The mixture, the molar ratio of 2,2-difluoroethanol to liquid ammonia is 1:5, and the liquid phase space velocity is 0.5h -1 , the residence time of 2,2-difluoroethanol was 44s, and the reaction yield was 82%.

[0031] Yield is defined as follows:

[0032] The mole percentage of the main raw material converted to the target product is used as the definition of the yield

[0033] Described catalyst comprises the component of following percentage by weight:

[0034]

[0035] The preparation method is as follows:

[0036] Using commercially available aluminum hydroxide as raw material, use 40% sodium hydroxide solution to make sodium metaaluminate solution, neutralize the precipitate with nitric acid, age, wash, f...

Embodiment 2

[0039] In a single-tube reactor with a diameter of 20mm, add 200ml of silicon oxide as a catalyst carrier, and under the conditions of a pressure of 0.8Mpa and a temperature of 175°C, and a hydrogen atmosphere, 2,2-difluoroethanol and liquid ammonia are introduced. The mixture, the molar ratio of 2,2-difluoroethanol to liquid ammonia is 1:8, and the liquid phase space velocity is 0.6h -1 , the residence time of 2,2-difluoroethanol was 37s, and the reaction yield was 79%.

[0040] Described catalyst comprises the component of following percentage by weight:

[0041]

[0042] The preparation method is the same as that in Example 1, and the carrier adopts commercially available silicon oxide.

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PUM

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Abstract

The invention discloses a preparation method of a 2,2-difluoroethylamine. The preparation method comprises the step of reacting 2,2-difluoroethanol with ammonia in hydrogen atmosphere in the presence of a catalyst, thereby obtaining the 2,2-difluoroethylamine. The method has the advantages that the reaction is carried out in a tubular fixed bed reactor at a lower pressure, the reaction conditions are mild and safe, the conversion rate and the yield of the reaction both are relatively high, few by-products are generated, continuous production can be realized easily, and the catalyst can be used for a long time and also can be regenerated.

Description

technical field [0001] The present invention relates to a process for 2,2-difluoroethylamine. Background technique [0002] 2,2-difluoroethanol is an important intermediate in the synthesis of important agrochemical and pharmaceutical active substances, especially for the preparation of 4-[(6-chloro-3-pyridylmethyl)( 2,2-Difluoroethyl)amino]furan-2(5H)-one is a novel insecticide. [0003] At present, there have been many patents and literatures reporting their respective technologies for preparing the 2,2-difluoroethanol, such as the technology disclosed in Chinese Patent Application No.: 201080033368.8, which includes the following steps: [0004] In a solvent with a maximum water content of 15% by volume, in the presence of a catalyst that accelerates the reaction with ammonia, a compound having the general formula CHF 2 -CH 2 The compound of Hal, wherein Hal is Cl, Br or I 2,2-difluoro-1-halogenated ethane reacts with ammonia to obtain the described 2,2-difluoroethylam...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/15C07C209/16B01J23/89
Inventor 王忠平刘纯山
Owner HUBEI HAIZHIJIE CHEM
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