反应详情

To a solution of 5-fluoro-3,4-dihydro-1H-quinoxalin-2-one from Example B (475 mg, 2.86 mmol) in THF (10 ml) was added sodium hydride (60%, 115 mg, 2.86 mg) while cooling in an ice/water bath. The mixture was allowed to warm to room temperature, stirred for 30 min and cooled in an ice/water bath. tert-Butyl bromoacetate (460 μl, 2.86 mmol) was added and the mixture was allowed to warm to room temperature slowly and stirred for 18 h. Brine was added and the mixture was evaporated in vacuo. The residue was partitioned between brine and EtOAc and the organic layer was dried and evaporated in vacuo. The residue was purified by flash chromatography on silica (eluant EtOAc;pet. ether 40:60) to give a white solid; yield 500 mg, 62%.

1. temperaturewhile cooling in an ice/water bath
2. temperaturecooled in an ice/water bath
3. temperatureto warm to room temperature slowly
4. stirringstirred for 18 h
5. customthe mixture was evaporated in vacuo
6. customThe residue was partitioned between brine and EtOAc
7. customthe organic layer was dried
8. customevaporated in vacuo
9. customThe residue was purified by flash chromatography on silica (eluant EtOAc;pet. ether 40:60)
10. customto give a white solid