反应详情

A solution of compound 1 (9.1 g, 25.5 mM) in THF (50 ml) was added over 45 min to a stirred suspension of LiAlH4 (0.726 g, 19.1 mM) in THF (50 ml) at 0° C. and stirring continued for 1 hr. The suspension was diluted with Et2O (100 ml) and H2O (0.73 ml), 15% aq. NaOH (0.73 ml) and H2O (2.1 ml) were added in sequence. The mixture was stirred for 16 hr, MgSO4 added and the suspension stirred an additional hour, filtered and the solids washed with Et2O. The combined organic layer was concentrated in vacuo, the residue dissolved inhot EtOAc and crystallized by the addition of hexane to give pure 3 (7.43 g, 93%) as a white solid, mp 95°-97° C., MS, m/e 314 (M+).

1. additionwere added in sequence
2. stirringThe mixture was stirred for 16 hr
3. stirringthe suspension stirred an additional hour
4. filtrationfiltered
5. washthe solids washed with Et2O
6. concentrationThe combined organic layer was concentrated in vacuo
7. dissolutionthe residue dissolved inhot EtOAc
8. customcrystallized by the addition of hexane