反应详情

To a solution of 2-amino-3-fluoro-N-methoxy-N-methyl-benzamide (765 mg, 3.86 mmol) in acetic acid (18 ml) was added 1,3-dichloro-5,5-dimethylimidazolidine-2,4-dione (783 mg, 2.7 mmol) at room temperature. The orange solution was stirred over night and was then poured carefully onto ice/saturated NaHCO3-solution. The mixture was extracted with EtOAc and the combined extracts were washed with brine, dried with Na2SO4 and evaporated. The remaining residue was purified by column chromatography (silica gel, heptane/EtOAc 90:10-80:20) to afford the title compound (544 mg, 61%) as light brown solid. MS (ESI): 233.0 (M+H)+.

1. additionwas then poured carefully onto ice/saturated NaHCO3-solution
2. extractionThe mixture was extracted with EtOAc
3. washthe combined extracts were washed with brine
4. dry with materialdried with Na2SO4
5. customevaporated
6. customThe remaining residue was purified by column chromatography (silica gel, heptane/EtOAc 90:10-80:20)