反应详情

To a mixture of 7-chloro-2,3-dihydro-4(lH)-quinolinone (20 g), pyridine (26 g) and dioxane (200 ml) was added dropwise 2-dimethylaminobenzoyl chloride (30 g) under cooling at 0° C. to 5° C. with stirring. The mixture was allowed to react at room temperature for additional 3 hours. The reaction mixture was poured into 500 ml of water, then shaken with additional dichloromethane (1000 ml). The organic layer was washed once with 1 N HCl (100 ml), twice with water (200 ml each) then once with saturated aqueous NaCl solution and dried over anhydrous sodium sulfate. Dichloromethane was removed in vacuo and the residue was recrystallized with dichloromethane and n-hexane to obtain 7-chloro-2,3-dihydro-l-(2-dimethylaminobenzoyl)-4(lH)-quinolinone (yield 35 g) as white crystal.

1. temperatureunder cooling at 0° C. to 5° C.
2. customto react at room temperature for additional 3 hours
3. washThe organic layer was washed once with 1 N HCl (100 ml), twice with water (200 ml each)
4. dry with materialonce with saturated aqueous NaCl solution and dried over anhydrous sodium sulfate
5. customDichloromethane was removed in vacuo
6. customthe residue was recrystallized with dichloromethane and n-hexane