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Preparing method of 1-cyclohexene ethylamine

A technology of cyclohexene ethylamine and cyclohexene acetonitrile, which is applied in the field of preparation of 1-cyclohexene ethylamine, can solve problems such as low yield and complex process, achieve high safety performance, optimize reaction process, and improve reaction Yield effect

Inactive Publication Date: 2016-06-15
ITIC MEDCHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Aiming at the deficiencies in the prior art, the present invention aims at the problem that the yield of 1-cyclohexeneethylamine is relatively low or the process is relatively complicated, and the rare metals hafnium, vanadium and niobium are added as catalysts. Stable properties, high reusability, can effectively reduce process costs, optimize the reaction process at the same time, simplify the reaction steps, and increase the reaction yield

Method used

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  • Preparing method of 1-cyclohexene ethylamine
  • Preparing method of 1-cyclohexene ethylamine
  • Preparing method of 1-cyclohexene ethylamine

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preparation example Construction

[0043] The preparation method of catalyst one to six is:

[0044] The first step: gradually add one or both of metal hafnium, vanadium and niobium into 5mol / L concentrated hydrochloric acid solution at a stirring speed of 1000 rpm, mix and stir for 5 minutes, then filter and remove the concentrated hydrochloric acid solution;

[0045] Step 2: Wash the catalyst with deionized water until it is neutral, then wash it with absolute ethanol for 2-3 times, and dry the catalyst for later use after the absolute ethanol washing is completed. The particle size of the catalyst is 10-20mm.

[0046] After the reaction, Agilent6890N gas chromatography was used for component analysis, and the chromatographic column was OV-101 capillary column and FID detector.

[0047] By adopting the catalyst of the invention, the yield of the reaction can be effectively improved, the generation of by-products can be reduced, and the economic benefit can be improved.

[0048] Experiment 2: Orthogonal anal...

Embodiment

[0058] Experimental steps of the embodiment of the present invention:

[0059] The first step: put 1-cyclohexene acetonitrile, methanol solvent, and dry catalyst into the reaction kettle;

[0060] Step 2: After sealing, first replace the air in the kettle with nitrogen, and then replace the nitrogen in the kettle with hydrogen;

[0061] The third step: heat up to the reaction temperature at a rate of 3°C / min, pass hydrogen to the reaction pressure, and keep the hydrogen pressure constant during the reaction;

[0062] Step 4: Stir the mixed materials, adjust the stirring speed to 500 rpm, and start timing the reaction until the end of the reaction.

[0063] Wherein, the catalyst preparation process comprises the following steps:

[0064] The first step: gradually add one or both of metal hafnium, vanadium and niobium to 5mol / L concentrated hydrochloric acid solution at a stirring speed of 1000 rpm, mix and stir for 5 minutes, then filter and remove the concentrated hydrochlor...

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Abstract

The invention discloses a preparing method of 1-cyclohexene ethylamine. 1-cyclohexene acetonitrile serves as a raw material for catalytic hydrogenation, a catalyst is one or two of hafnium, vanadium and niobium, the particle size of the catalyst is 10-20mm, reaction temperature is 1200-1300 DEG C, reaction pressure is 1.1-1.2MPa, a reaction stirring speed is 500 revolutions / minute, reaction time is 2.0-3.0h, under the reaction conditions, the yield of the 1-cyclohexene ethylamine is 70% or more, the method is simple in step and easy to operate, a reaction system is high in safety performance, processing cost is low, the yield is higher and economic values are better.

Description

Technical field: [0001] The invention relates to a preparation method of 1-cyclohexeneethylamine, which belongs to the field of chemical synthesis. Background technique: [0002] 1 Cyclohexeneethylamine is an important pharmaceutical intermediate, which is used as a raw material for antitussives and analgesics such as Kemiphen and Temaren, so the preparation of this substance is of great significance. There are many ways to prepare 1 cyclohexeneethylamine, such as direct catalytic hydrogenation, reduction of dissolved metals, reduction of complex metal hydrides, etc. [0003] Preparation of 1-cyclohexeneethylamine by indirect method, first prepare cyclohexene acetic acid by hydrolysis of 1-cyclohexene acetonitrile, prepare cyclohexene acetyl chloride from cyclohexene acetic acid, and then convert cyclohexene acetyl chloride into cyclohexene ethanol 1. Cyclohexene ethanol is prepared to obtain 2-(cyclohexenyl)-chloroalkane, and finally 2-(cyclohexenyl)-chloroalkane is oxidiz...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/48C07C211/25B01J21/06B01J23/20B01J23/22
CPCB01J21/066B01J23/20B01J23/22C07C209/48C07C211/25
Inventor 胡海威丁靓闫永平郑辉严辉
Owner ITIC MEDCHEM CO LTD