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
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[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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