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Method for producing 4-N,N-dimethylamino methylaniline

A technology of dimethylaminomethylaniline and nitrobenzene, which is applied in the field of organic compound synthesis, can solve problems to be improved and the like, and achieves the effects of being suitable for large-scale production, mild reaction conditions and high product yield

Inactive Publication Date: 2010-06-16
大连凯飞精细化工有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] 4-N,N-Dimethylaminomethylaniline is an important medicinal chemical intermediate. Due to the application requirements, the obtained product is required to have high purity, and the current large-scale industrial production still needs to be improved to meet the huge application requirements.

Method used

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  • Method for producing 4-N,N-dimethylamino methylaniline

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Embodiment 1

[0013] The compound nitrobenzene (12.87g, 0.0715mol) was dissolved in 56ml of ethanol, 1% Rany Ni was added thereto, and the hydrogen pressure was kept at 1 atm, and the mixture was stirred for 2 days at a temperature of 80°C. After the reaction was completed, the reaction solution was filtered and concentrated, and distilled under reduced pressure to obtain 9.7 g of a light yellow liquid 4-N,N-dimethylaminomethylaniline, with a yield of 90%.

Embodiment 2

[0015] The compound nitrobenzene (12.87 g, 0.0715 mol) was dissolved in 56 ml of methanol, 10% Rany Ni was added thereto, and the hydrogen pressure was kept at 0.5 atm, and the mixture was stirred for 6 hours at a temperature of 70°C. After the reaction was completed, the reaction solution was concentrated by filtration and concentrated under reduced pressure to obtain 9.9 g of a light yellow liquid 4-N,N-dimethylaminomethylaniline, with a yield of 92%.

Embodiment 3

[0017] Compound nitrobenzene (12.87g, 0.0715mol) was dissolved in 56ml of isopropanol, 20% Rany Ni was added thereto, and the pressure of hydrogen was maintained at 0.1-1 atm. When the temperature was 30°C, it was stirred for 36 hours. After the reaction was completed, the reaction solution was filtered and concentrated, and distilled under reduced pressure to obtain 10.1 g of a light yellow liquid 4-N,N-dimethylaminomethylaniline, with a yield of 94%.

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Abstract

The invention relates to a composite method of organic compounds, in particular to a method for producing 4-N,N-dimethylamino methylaniline. Raw material nitrobenzene is dissolved in organic solvent, Raney nickel is added at the weight ratio of 1-20% of catalyst to nitrobenzene; hydrogen is introduced in, and hydrogen pressure is kept under 0.1-1 atm; when temperature is 20-80 DEG C, the mixture is stirred for 6-48 hours for reacting; after reaction ends, reaction liquid is filtered and concentrated to obtain the 4-N,N-dimethylamino methylaniline. The invention uses the Raney Nickel to catalyze, hydrogenate and reduce nitrobenzene derivant 4-N, N-dimethylamino methylaniline. The invention has simple technical step, quick one-step reaction, moderate reaction condition, easy operation and no pollution; the product has high yield and high purity, is suitable to be produced on large scale and satisfies the application requirements of pharmaceuticals industry and the like.

Description

Technical field: [0001] The present invention relates to a method for synthesizing organic compounds. Background technique: [0002] 4-N,N-Dimethylaminomethylaniline is an important medicinal chemical intermediate. Due to the application requirements, the obtained product is required to have high purity, and the current large-scale industrial production still needs to be improved to meet the huge application requirements. . Invention content: [0003] The purpose of this invention is to provide a kind of method of producing 4-N, N-dimethylaminomethylaniline, reacts rapidly, and technique is simple. [0004] The technical solution adopted by the present invention for realizing the above object is: produce 4-N, the method for N-dimethylaminomethylaniline, raw material nitrobenzene is dissolved in the organic solvent, is 1 by catalyst and nitrobenzene weight ratio Raney nickel is added thereto at a ratio of -20%, hydrogen gas is introduced and the pressure of the hydrogen g...

Claims

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Application Information

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IPC IPC(8): C07C211/49C07C209/36
Inventor 王乃伟姜人武孙玉琴秦学孔
Owner 大连凯飞精细化工有限公司
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