反应详情

20 g of 5-chloroindan-1-one are dissolved in 600 ml of dry toluene and, after addition of 27.4 ml of N,N-dimethylhydrazine and 1 g of p-toluenesulfonic acid, boiled with a water trap for 4 h. The reaction mixture is concentrated in vacuo, and the residue is dissolved in ethyl acetate and washed with sodium bicarbonate solution and then with water. The organic phase is dried over sodium sulfate and concentrated in vacuo, and the residue is chromatographed on silica gel with ethyl acetate/heptane ½. N′-(5-chloroindan-1-ylidene)-N,N-dimethylhydrazine is obtained as an oil.

1. concentrationThe reaction mixture is concentrated in vacuo
2. dissolutionthe residue is dissolved in ethyl acetate
3. washwashed with sodium bicarbonate solution
4. dry with materialThe organic phase is dried over sodium sulfate
5. concentrationconcentrated in vacuo
6. customthe residue is chromatographed on silica gel with ethyl acetate/heptane ½