反应详情

温度

160 °C

A mixture of 9-bromo-5-methoxycarbonylmethyl-6,7-dihydro-1H, 5H-pyrido[1,2,3-de]quinoxaline-2,3-dione (530 mg, 1.50 mmol) and cuprous chloride (1.0 g, 10.1 mmol) in dimethyl sulfoxide (5 mL) was heated at 160° C. for 4.5 h and poured into 1N aqueous ammonium chloride (200 mL). The mixture was extracted with a mixed solvent of THF and ethyl acetate (600 mL). The extract was washed with 1N aqueous ammonium chloride (200 mL×2) and brine (200 mL), dried over magnesium sulfate, and concentrated. The residue was recrystallized from ethanol to give 125 mg of the title compound (27%).

1. extractionThe mixture was extracted with a mixed solvent of THF and ethyl acetate (600 mL)
2. washThe extract was washed with 1N aqueous ammonium chloride (200 mL×2) and brine (200 mL)
3. dry with materialdried over magnesium sulfate
4. concentrationconcentrated
5. customThe residue was recrystallized from ethanol