反应详情

H2SO4 (1.5 equiv.) was added to a suspension of LAH (3 equiv.) in THF (32 ml) at 0° C. and the mixture was stirred at room temperature for 0.5 h. A solution of 1-benzyl-4-(4-(pyridin-4-yl)piperazin-1-yl)piperidine-4-carbonitrile (5.54 mmol, 1 equiv.) in THF was added under cooled conditions and the resulting reaction mixture was heated to 50° C. for 16 h. The reaction was quenched with THF/H2O solution, filtered and the solid residue washed with excess ethyl acetate. The organic layer was given a brine wash, dried over sodium sulfate and the solvent was removed under reduced pressure. The resulting crude product was used for the next step without further purification. Yield: 85%.

1. customthe resulting reaction mixture
2. temperaturewas heated to 50° C. for 16 h
3. customThe reaction was quenched with THF/H2O solution
4. filtrationfiltered
5. washthe solid residue washed with excess ethyl acetate
6. washwash
7. dry with materialdried over sodium sulfate
8. customthe solvent was removed under reduced pressure
9. customThe resulting crude product was used for the next step without further purification