反应详情

To a stirred suspension of 6 (1.92 g, 9 mmol) in dry DMF (100 mL) at 0° C., NaH (0.43 g, 18 mmol) was added and the mixture was stirred at room temperature for 1 h. Ethyl bromoacetate (1.5 g, 9 mmol) was added dropwise at 0° C. and stirred for 1 h. Methanol (2 mL) was added to quench the reaction, and the solvents were removed under reduced pressure. The residue obtained was dissolved in DCM, washed with water (3×50 mL), dried over Na2SO4, and the solvent was evaporated to give 7 as a white solid (1.38 g, 54%).

1. stirringstirred for 1 h
2. customto quench
3. customthe reaction
4. customthe solvents were removed under reduced pressure
5. customThe residue obtained
6. washwashed with water (3×50 mL)
7. dry with materialdried over Na2SO4
8. customthe solvent was evaporated