反应详情

A solution of 29 (1.2 g, 2.27 mmol) in acetonitrile (70 mL) and 50% aqueous hypophosphorous acid (30 mL) was kept at reflux for 3.5 hr. The acetonitrile was removed in vacuo, the residue was diluted with ethyl acetate (150 mL) and water (100 mL). Phases were separated. The organic phase was washed with saturated sodium bicarbonate (2×100 mL) and water (100 mL), dried over sodium sulfate and filtered. The solvent was removed on a rotary evaporator. The crude product was purified by chromatography on silica (45 g) with hexane (2 L) to yield pure D4 (0.92 g, 96%).

1. temperatureat reflux for 3.5 hr
2. customThe acetonitrile was removed in vacuo
3. additionthe residue was diluted with ethyl acetate (150 mL) and water (100 mL)
4. customPhases were separated
5. washThe organic phase was washed with saturated sodium bicarbonate (2×100 mL) and water (100 mL)
6. dry with materialdried over sodium sulfate
7. filtrationfiltered
8. customThe solvent was removed on a rotary evaporator
9. customThe crude product was purified by chromatography on silica (45 g) with hexane (2 L)