反应详情

To 141D (6.7 g; 13.25 mmol) in dichloromethane (80 mL) was added sodium bicarbonate (132 mL, 1 M). Benzyl chloroformate (1.89 mL, 13.25 mmol) in dichloromethane (20 mL) was then added dropwise using an addition funnel over a period of 1 h. After the addition was complete, the suspension turned to a clear orange solution. The layers were separated and the organic layer was washed with brine and dried over sodium sulfate. The solvent was removed and the crude residue was purified by flash column chromatography to give 4.6 g of 141E as a yellow solid (69% yield). LC-MS: 520.10 (M+H)+.

1. customof 1 h
2. additionAfter the addition
3. customThe layers were separated
4. washthe organic layer was washed with brine
5. dry with materialdried over sodium sulfate
6. customThe solvent was removed
7. customthe crude residue was purified by flash column chromatography