反应详情

温度

0 °C

10.8 g (201 mmol) of ammonium chloride are suspended in 200 ml of dry toluene and the suspension is cooled to 0° C. 100 ml of a 2M solution of trimethylaluminium in hexane are added dropwise and the mixture is stirred at room temperature until the evolution of gas is complete. After addition of 13.2 g (100 mmol) of 4-methylbenzyl cyanide, the reaction mixture is stirred overnight at 80° C. (bath). The cooled reaction mixture is treated with ice-cooling with 35 ml of methanol and then stirred at room temperature for a further 1 h. The solid is then first filtered off with suction, and the filter cake is washed several times with methanol. The filtrate is concentrated, the residue is resuspended in dichloromethane/methanol 10/1 and the insoluble solid is separated off. The filtrate is then again evacuated from the solvent in vacuo.

1. stirringthe reaction mixture is stirred overnight at 80° C. (bath)
2. customThe cooled reaction mixture
3. additionis treated with ice-
4. stirringstirred at room temperature for a further 1 h
5. filtrationThe solid is then first filtered off with suction
6. washthe filter cake is washed several times with methanol
7. concentrationThe filtrate is concentrated
8. customthe insoluble solid is separated off
9. customThe filtrate is then again evacuated from the solvent in vacuo