Production method for 1,2-N,N'dimethylcyclohexanediamine

A technology of dimethylcyclohexanediamine and its production method, which is applied in 1 field, can solve problems such as difficult separation, high price, and danger of lithium aluminum hydride, and achieve the effect of good product selectivity and easy operation

Inactive Publication Date: 2012-10-17
姜树林
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  • Summary
  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Existing 1,2-N, the production method of N` dimethylcyclohexanediamine, such as: Journal of the American Chemical Society, 124 (39), 11684-11688; 2002 is based on cyclohexanediamine and chloroform Ester reaction or formate rea

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Step 1: Sulfonation of Cyclohexanediamine

[0013] Dissolve 1,2-cyclohexanediamine (20mmol) in 10ml of pyridine, add the above solution dropwise to a solution of p-toluenesulfonyl chloride (40mmol) in pyridine (10ml), and control the temperature below 60 during the dropping process. The color of the solution changed from colorless to dark red. After dropping, put it at room temperature to react for 7 hours, stop the reaction, add 15% hydrochloric acid to adjust the pH to 6-7, let it stand overnight, filter, wash with water (10ml*3), and obtain 6.5g of white powdery solid,

[0014] Step 2: Methylation

[0015] The product of step 1 (7.18 mmol) was dissolved in acetonitrile (60 ml), potassium carbonate (28.7 mmol) powder was added, and stirred at room temperature for 1 h. Place in ice bath and add iodomethane (28.7mmol), react in ice bath for 30min, remove the ice bath and react at room temperature for 12h. Stop the reaction, remove acetonitrile by rotary evaporation, ...

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PUM

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Abstract

The present invention discloses a production method for 1,2-N,N'dimethylcyclohexanediamine. According to the method, N single protection is performed on o-phenylene diamine and aromatic benzene sulfonyl chloride; methyl iodide or dimethyl sulphate is adopted to carry out a N methylation reaction; N single protection is performed on 1,2-diaminocyclohexane and aromatic benzene sulfonyl chloride, then methyl iodide or dimethyl sulphate is adopted to carry out a N methylation reaction, a hydrolysis reaction is performed in the presence of sulphuric acid to remove aromatic benzenesulfonyl to obtain the target product 1,2-N,N'dimethylcyclohexanediamine. The process of the present invention is simple and easy to operate, and the high purity target product can be obtained with the method of the present invention.

Description

technical field [0001] The present invention relates to a kind of 1,2-N, the production method of N' dimethylcyclohexanediamine. Background technique [0002] Existing 1,2-N, the production method of N` dimethylcyclohexanediamine, such as: Journal of the American Chemical Society, 124 (39), 11684-11688; 2002 is based on cyclohexanediamine and chloroform Ester reaction or formate ester reaction, then reduction reaction with lithium aluminum hydride, the raw material is not only expensive, but also very dangerous to use lithium aluminum hydride, the resulting product has poor selectivity and is difficult to separate. Our method is to avoid strong reducing agents and dangerous processes, and find a process route that is more suitable for industrialization, and can obtain target products with higher purity. Contents of the invention [0003] The purpose of the present invention is to provide a simple process, which can obtain the target product with high purity, and does not ...

Claims

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Application Information

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IPC IPC(8): C07C211/36C07C209/68
Inventor 王德峰石飞朱小飞王炳才张耀斌俞健钧
Owner 姜树林
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