反应详情

A solution of 26 (0.85 g, 1.55 mmol) in acetonitrile (50 mL) and 50% aqueous hypophosphorous acid (21 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 (80 mL). Phases were separated. The organic phase was washed with saturated sodium bicarbonate (2×80 mL) and water (2×80 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 2% ethyl acetate in heptane (4 L) to yield pure D2 (0.42 g, 69%).

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 (80 mL)
4. customPhases were separated
5. washThe organic phase was washed with saturated sodium bicarbonate (2×80 mL) and water (2×80 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 2% ethyl acetate in heptane (4 L)