反应详情

A mixture of 5-(4-fluoro-benzyloxy)-isoindole-1,3-dione (100 mg, 0.37 mmol), sodium hydride (55% in mineral oil, 18 mg, 0.42 mmol) and 2-bromoacetamide (61 mg, 0.44 mmol) in dry tetrahydrofuran (5 mL) at 0° C. was stirred at room temperature for 3 h and then heated at 50° C. for 1 h. After cooling to 0° C., water (2 mL) was added and the product extracted with ethyl acetate. The organic extracts were then washed with brine and dried over sodium sulfate. Filtration and evaporation gave a residue which was purified by chromatography (SiO2, heptane-CH2Cl2 2:3 then CH2Cl2— 2N NH3-MeOH 99:1: to 4:1) to afford the title compound (78 mg, 65%) as a white solid.

1. temperatureheated at 50° C. for 1 h
2. temperatureAfter cooling to 0° C.
3. extractionthe product extracted with ethyl acetate
4. washThe organic extracts were then washed with brine
5. dry with materialdried over sodium sulfate
6. filtrationFiltration and evaporation
7. customgave a residue which
8. customwas purified by chromatography (SiO2, heptane-CH2Cl2 2:3