反应详情

A mixture of 19 (1.9 g, 4.6 mmol), 20% Pd—C (˜55% H2O) and EtOH (50 mL) was hydrogenated at 20 psi H2 for 2 hr at which time LCMS show no 19 remained. The mixture was filtered through Celite, washing the Celite pad with EtOH (100 mL). The filtrate was concentrated under reduced pressure to give a yellow-green oil. The crude product was purified on an Analogic MPLC, eluting with a gradient of 0%-20% EtOAc/hexanes to give 0.9 g (60%) of D1 as a faintly yellow viscous oil. On lengthy standing (>2 months) D1 slowly crystallized as a white solid (mp 116.0-116.8° C.).

1. filtrationThe mixture was filtered through Celite
2. washwashing the Celite pad with EtOH (100 mL)
3. concentrationThe filtrate was concentrated under reduced pressure
4. customto give a yellow-green oil
5. customThe crude product was purified on an Analogic MPLC
6. washeluting with a gradient of 0%-20% EtOAc/hexanes