反应详情

温度

0 °C

To a solution of Intermediate 51 (7.51 g, 19.54 mmol) in THF (500 ml) at 0° C. was added NaH (1.172 g, 29.3 mmol) portionwise. The mixture was stirred at 0° C. for 3 hrs, then benzenesulfonyl chloride (3.70 ml, 25.4 mmol) was added and stirring was continued at r.t. overnight. The reaction mixture was quenched with sat. aqueous NH4Cl solution, and extracted with EtOAc. The organic layer was dried, filtered, and evaporated to dryness. Purification by flash chromatography (silica gel, cyclohexane/EtOAc gradient) yielded Intermediate 52.

1. stirringstirring
2. waitwas continued at r.t. overnight
3. customThe reaction mixture was quenched with sat. aqueous NH4Cl solution
4. extractionextracted with EtOAc
5. customThe organic layer was dried
6. filtrationfiltered
7. customevaporated to dryness
8. customPurification by flash chromatography (silica gel, cyclohexane/EtOAc gradient)