反应详情

A solution of 3-(2-methyl-1,3-dioxolan-2-yl)benzonitrile (65.6 g) in tetrahydrofuran (400 ml) was added to a suspension of lithium aluminum hydride (26.3 g) in tetrahydrofuran (400 ml) with cooling on an ice-water bath under nitrogen stream for 1 hour. The mixture was stirred at room temperature for 2 hours. Ethyl acetate (200 ml) was added slowly with cooling on an ice bath and then ice-water (200 ml) was added very slowly with cooling on an ice bath. The resulting precipitate was removed by filtration. The solvent was removed under reduced pressure. Chloroform (300 ml) was added to the residue. The mixture was washed with water (100 ml) and then dried with magnesium sulfate. The solvent was removed under reduced pressure to afford 3-(2-methyl-1,3-dioxolan-2-yl)benzylamine (57.2 g) (oil).

1. temperaturewith cooling on an ice-water bath under nitrogen stream for 1 hour
2. temperaturewith cooling on an ice bath
3. temperaturewith cooling on an ice bath
4. customThe resulting precipitate was removed by filtration
5. customThe solvent was removed under reduced pressure
6. additionChloroform (300 ml) was added to the residue
7. washThe mixture was washed with water (100 ml)
8. dry with materialdried with magnesium sulfate
9. customThe solvent was removed under reduced pressure