反应详情

To a mixture of benzaldehyde (425 mg, 4.0 mmol), aniline (372 mg, 4.0 mmol) and acetonitrile (8 ml) were added N-Boc-3-methyldihydropyrrole (732 mg, 4.0 mmol) and Dy(OTf)3 (122 mg, 0.19 mmol) under ice-cooling, and the mixture was stirred at the same temperature for 30 min., and at room temperature for 1 hr. The reaction mixture was concentrated under reduced pressure, water was added and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, dried (over anhydrous MgSO4), and concentrated under reduced pressure. The residue was subjected to column chromatography using silica gel (30 g) and eluted with hexane-ethyl acetate (4:1, v/v) to give the title compound (780 mg, 53%) as an amorphous form.

1. temperaturecooling
2. waitat room temperature for 1 hr
3. concentrationThe reaction mixture was concentrated under reduced pressure, water
4. additionwas added
5. extractionthe mixture was extracted with ethyl acetate
6. washThe extract was washed with saturated brine
7. dry with materialdried (over anhydrous MgSO4)
8. concentrationconcentrated under reduced pressure
9. washeluted with hexane-ethyl acetate (4:1