反应详情

温度

0 °C

21.4 g (400 mmol) of ammonium chloride are suspended in 375 ml of toluene, and the suspension is cooled to 0° C. 200 ml of a 2 M solution of trimethylaluminum in hexane are added dropwise, and the mixture is stirred at room temperature until the evolution of gas has ceased. Following addition of 29.44 g (200 mmol) of 2-ethoxybenzonitrile, the reaction mixture is stirred at 80° C. (bath) overnight. The cooled reaction mixture is, with ice-cooling, added to a suspension of 100 g of silica gel and 950 ml of chloroform, and the mixture is stirred at room temperature for 30 minutes. The mixture is filtered off with suction and the filter cake is washed with the same amount of methanol. The mother liquor is concentrated, the resulting residue is triturated with a mixture of dichloromethane and methanol (9:1), the solid is filtered off with suction and the mother liquor is concentrated. This gives 30.4 g (76%) of a colorless solid.

1. stirringthe reaction mixture is stirred at 80° C. (bath) overnight
2. customThe cooled reaction mixture
3. temperaturecooling
4. stirringthe mixture is stirred at room temperature for 30 minutes
5. filtrationThe mixture is filtered off with suction
6. washthe filter cake is washed with the same amount of methanol
7. concentrationThe mother liquor is concentrated
8. customthe resulting residue is triturated with a mixture of dichloromethane and methanol (9:1)
9. filtrationthe solid is filtered off with suction
10. concentrationthe mother liquor is concentrated