反应详情

温度

0 °C

To a solution of Intermediate 53 (3.82 g, 6.33 mmol) in THF (64 ml) was added a solution of potassium tert-butylate in THF (1 M, 9.49 ml, 9.49 mmol) at 0° C. The mixture was stirred at 0° C. for 1 hr, then an additional solution of potassium tert-butylate in THF (1 M, 2.00 ml, 2.00 mmol) was added and stirring was continued for an additional 1 hr. The reaction was quenched by addition of sat. aqueous NaHCO3 solution, and the mixture was extracted with EtOAc. The organic layer was dried, filtered, and evaporated to dryness. Purification by flash chromatography (silica gel, cyclohexane/EtOAc gradient) yielded Intermediate 54.

1. stirringstirring
2. waitwas continued for an additional 1 hr
3. customThe reaction was quenched by addition of sat. aqueous NaHCO3 solution
4. extractionthe mixture was extracted with EtOAc
5. customThe organic layer was dried
6. filtrationfiltered
7. customevaporated to dryness
8. customPurification by flash chromatography (silica gel, cyclohexane/EtOAc gradient)