Method of preparing N-ethyl-N-cyanoethyl aniline

A technology of cyanoethylaniline and ethylaniline, which is applied in the field of preparation of N-ethyl-N-cyanoethylaniline, can solve the problem of high preparation cost and achieve the effect of increasing selectivity and reducing production cost

Active Publication Date: 2008-11-19
内蒙古美力坚科技化工有限公司
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Problems solved by technology

[0012] In the above-mentioned preparation process, in the condensation reaction step, the selectivity of N-ethylaniline only reaches 60%, and the preparation cost of N-ethyl-N-cyanoethylaniline is high

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Embodiment Construction

[0022] The specific implementation of the present invention will be described below:

[0023] The preparation method of N-ethyl-N-cyanoethylaniline of the present invention mainly includes the following steps:

[0024] ① Condensation reaction: Into a 1L autoclave equipped with stirring and a thermometer, add 235 grams of aniline, 145 grams of ethanol, 8.5 grams of phosphorus oxychloride and 2 grams of phosphorus trichloride mixed catalyst, and slowly increase the temperature to 230~ 240°C, gauge pressure of 3~3.5MP, reaction for 10 hours.

[0025] The product of the condensation reaction was analyzed by gas chromatography. Among them, aniline was 26%, N-ethylaniline was 68%, and N,N-diethylaniline was 5 to 6%.

[0026] ② Distillation: Collect the first fraction as aniline under the conditions of vacuum 0.1MP and temperature less than 135℃, collect the second fraction as N-ethylaniline at 145℃, and collect the third fraction at 145~148℃ It is N,N-diethylaniline. Finally, 78 grams o...

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Abstract

The invention relates to a method for preparing N-ethide-N-cyanoethyl aniline, mainly comprising the following: (1) a step of condensation reaction, during which, aniline reacts with ethanol in the action of catalyst to generate N-ethyl aniline and N, N- diethylaniline which are separated through distillation to produce pure N-ethyl aniline; (2) a step of addition reaction, during which, the pure N-ethyl aniline obtained in the step (1) reacts with acrylonitrile in the action of the catalyst to produce the N-ethide-N-cyanoethyl aniline; particularly, the condensation reaction is performed in the action of a binary catalyst formed by any two of phosphorus oxychloride, phosphorus trichloride, phosphorus pentachloride, phosphorus trichloride and inorganic acid, and the content of one composition of the binary catalyst is between 5 and 95 percent. In the preparing process, on the basis of the prior process, the binary catalyst is used in the condensation reaction; and the reaction selectivity is improved and the production cost is lowered without changing the reaction condition and so on.

Description

Technical field [0001] The invention relates to a preparation method of N-ethyl-N-cyanoethyl aniline. Background technique [0002] N-ethyl-N-cyanoethyl aniline is mainly used in the synthesis of disperse dyes, and is the main intermediate for the manufacture of disperse yellow, brown, red and other chromatograms. [0003] In the prior art, the preparation process of N-ethyl-N-cyanoethylaniline mainly includes the following steps: [0004] (A), condensation reaction [0005] Under the action of catalyst and pressure from aniline and ethanol, N-ethylaniline and N,N-diethylaniline are produced. The choice of catalyst can be hydrochloric acid, sulfuric acid, phosphorus oxychloride and other compounds. The reaction temperature is 230-250°C, the gauge pressure is 3-4.5MPa, and the reaction time is about 10 hours. The resulting product has an aniline content of 28-31%; N -The content of ethylaniline is 58-60%; the content of N,N-diethylaniline is 8-10%. [0006] (B), distillation [00...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/25C07C253/30B01J27/14
Inventor 倪惠林潘培华张正富蔡元良
Owner 内蒙古美力坚科技化工有限公司
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