反应详情

温度

0 °C

To a solution of the subtitle product of step iv) (0.50 g) in DMF (10 ml) was added tert-butyldimethylsilyl chloride (0.51 g) at −10° C. in portions. To this mixture was then added imidazole in portions. The mixture was then stirred at 0° C. for 1 h and allowed to come to room temperature and stirred for 16 h. The mixture was quenched with water and extracted with EtOAc (2×250 ml). The combined organics were washed with water (3×20 ml) and brine (3×20 ml), the organic layer dried (MgSO4) and the solid filtered. The filtrate was evaporated to dryness and the residue chromatographed on silica gel eluting with EtOAc/isohexane (1:1) to yield the subtitle compound as an oil. Yield 1.0 g.

1. customto come to room temperature
2. stirringstirred for 16 h
3. customThe mixture was quenched with water
4. extractionextracted with EtOAc (2×250 ml)
5. washThe combined organics were washed with water (3×20 ml) and brine (3×20 ml)
6. dry with materialthe organic layer dried (MgSO4)
7. filtrationthe solid filtered
8. customThe filtrate was evaporated to dryness
9. customthe residue chromatographed on silica gel eluting with EtOAc/isohexane (1:1)