反应详情

A solution of D1 (11.5 g, 0.04 mol) in DCM (80 ml) was cooled (ice-bath) and TFA (excess, 50ml) was added. Reaction was warmed to ambient temperature, stirred for 3 h and partitioned between ethyl acetate and aqueous sodium hydroxide. The organic phase was separated, dried (MgSO4) and filtered. Removal of solvent under reduced pressure afforded the crude product as a yellow oil. Bulb to bulb distillation under reduced pressure initially afforded the product as a oil which crystallised on standing.

1. additionwas added
2. customReaction
3. custompartitioned between ethyl acetate and aqueous sodium hydroxide
4. customThe organic phase was separated
5. dry with materialdried (MgSO4)
6. filtrationfiltered
7. customRemoval of solvent under reduced pressure
8. customafforded the crude product as a yellow oil
9. distillationBulb to bulb distillation under reduced pressure