反应详情

温度

80 °C

AlCl3 (500 g, 3.8 mol) was carefully added to a suspension of 3-methyl-but-2-enoic acid phenylamide (105 g, 0.6 mol) in benzene (1000 mL). The reaction mixture was stirred at 80° C. overnight and poured into ice-water. The organic layer was separated and the aqueous layer was extracted with ethyl acetate (250 mL×3). The combined organic layers were washed with water (200 mL×2) and brine (200 mL), dried over Na2SO4 and concentrated to give 4,4-dimethyl-3,4-dihydro-1H-quinolin-2-one (90 g, 86%).

1. customThe organic layer was separated
2. extractionthe aqueous layer was extracted with ethyl acetate (250 mL×3)
3. washThe combined organic layers were washed with water (200 mL×2) and brine (200 mL)
4. dry with materialdried over Na2SO4
5. concentrationconcentrated