反应详情

温度

80 °C

A mixture of (2) (1.98 g, 10.0 mmol), ammonium acetate (23.2 g, 300 mmol), and sodium cyanoborohydride (4.63 g, 69.9 mmol) in EPA (100 mL) was heated at 80° C. overnight. The mixture was evaporated under reduced pressure to remove IPA. The residue was diluted with water, and basified with NaOH (2M) to pH>7. The aqueous layer was extracted with dichloromethane (3×). The pooled organic layer was removed under vacuum. The residue was purified by chromatography on silica gel (100% ethyl acetate, then 10% saturated ammonia methanol in dichloromethane) to give 1-phenyl-2-(pyridin-4-yl)ethanamine (3) as a clear oil (0.780 g, 3.94 mmol, 39% yield).

1. customThe mixture was evaporated under reduced pressure
2. customto remove IPA
3. additionThe residue was diluted with water
4. extractionThe aqueous layer was extracted with dichloromethane (3×)
5. customThe pooled organic layer was removed under vacuum
6. customThe residue was purified by chromatography on silica gel (100% ethyl acetate