反应详情

To a stirred solution of compound (2) (4.69 g, 20.66 mmol) and imidazole (2.10 g, 30.99 mmol) in dry DMF (100 mL) was added TBDMSCl (4.70 g, 30.99 mmol). After 16 hr, further aliquots of imidazole (2.10 g, 30.99 mmol) and TBDMSCl (4.70 g, 30.99 mmol) were added and the mixture was stirred for 48 hr. The reaction mixture was diluted with water (120 mL) and extracted with DCM (2×200 mL). The combined organic extracts were washed with water (2×200 mL), dried, filtered and the volume reduced to approximately 100 mL by evaporation in vacuo. The resulting slurry was filtered and the solid washed with heptane (50 mL) to afford the title compound (3) (6.05 g, 85%) as an off-white solid: m/z 343 (M+H)+ (ES+).

1. extractionextracted with DCM (2×200 mL)
2. washThe combined organic extracts were washed with water (2×200 mL)
3. customdried
4. filtrationfiltered
5. customthe volume reduced to approximately 100 mL by evaporation in vacuo
6. filtrationThe resulting slurry was filtered
7. washthe solid washed with heptane (50 mL)