反应详情

温度

23 °C

Palladium acetate (129 mg, 0.57 mmol) was added to a suspension of silver carbonate (1.6 g, 5.72 mmol), 1,3-bis(diphenylphosphino)propane (236 mg, 0.57 mmol), tributylphosphine (0.713 ml, 579 mg, 2.86 mmol) and N-ethyl-2-bromo-5-nitro-N-phenyl-benzamide (1.0 g, 2.86 mmol) in DMF (15 ml). The reaction mixture was heated to reflux for 30 minutes and cooled to 23° C. The mixture was filtered through a plug of celite, and the filter cake was washed with ethyl acetate (50 ml). The combined filtrates were washed with saturated sodium chloride (3-30 ml portion), dried over anhydrous sodium sulfate, and were concentrated. The residue was purified by flash column chromatography (10% ethyl acetate in dichloromethane) afforded 5-ethyl-8-nitro-5H-phenanthridin-6-one I-16b (111 mg, 14%) as a yellow solid.

1. temperatureThe reaction mixture was heated
2. temperatureto reflux for 30 minutes
3. filtrationThe mixture was filtered through a plug of celite
4. washthe filter cake was washed with ethyl acetate (50 ml)
5. washThe combined filtrates were washed with saturated sodium chloride (3-30 ml portion)
6. dry with materialdried over anhydrous sodium sulfate
7. concentrationwere concentrated
8. customThe residue was purified by flash column chromatography (10% ethyl acetate in dichloromethane)