反应详情

温度

0 °C

Mix lithium aluminum hydride (1.0 g, 26.6 mmol) and anhydrous ethyl ether (70 mL) under nitrogen atmosphere. Stir and cool to 0° C. in an ice bath. Add dropwise a solution of 4-(3,3-dimethylbutoxy)-benzonitrile (1.8 g, 8.87 mmol) in anhydrous ethyl ether (20 mL). Stir for 2 h at 0° C., remove the ice bath and stir at ambient temperature for 18 h. Cool the reaction flask in an ice bath and add carefully dropwise and sequentially water (1 mL), 2N aqueous NaOH (1 mL), and water (2 mL). Stir for 30 min. filter, separate the organic layer, dry over Na2SO4 and concentrate in vacuo to obtain the title compound (1.62 g, 88%). MS (ES+) m/z: 191 M+H−NH3)+.

1. stirringStir for 2 h at 0° C.
2. customremove the ice bath
3. stirringstir at ambient temperature for 18 h
4. temperatureCool the reaction flask in an ice bath
5. additionadd carefully dropwise
6. stirringStir for 30 min.
7. filtrationfilter
8. customseparate the organic layer
9. dry with materialdry over Na2SO4
10. concentrationconcentrate in vacuo