反应详情

温度

60 °C

To a solution of ethyl 3-(dimethylamino)-2-(2-fluoro-5-iodobenzoyl)acrylate (Intermediate 24, 1 g, 2.56 mmol) dissolved in THF (10 mL) was added (R)-2-aminopropan -1-ol (300 mg, 2.56 mmol). The reaction mixture was stirred at 60° C. for 2 h. The reaction mixture was concentrated under reduced pressure, and the resulting residue was suspended in DMF (10 mL). Potassium carbonate was added (1.06 g, 7.67 mmol, 3 equiv.), and the reaction mixture was stirred at 70° C. for 18 h. The reaction mixture was cooled down to room temperature and quenched with 1 N HCl. The precipitate that formed was collected by filtration, washed with water and hexanes to provide (R)-ethyl 1-(1-hydroxypropan-2-yl)-6-iodo-4-oxo-1,4-dihydroquinoline-3-carboxylate (446 mg, 39%).

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. additionPotassium carbonate was added (1.06 g, 7.67 mmol, 3 equiv.)
3. stirringthe reaction mixture was stirred at 70° C. for 18 h
4. temperatureThe reaction mixture was cooled down to room temperature
5. customquenched with 1 N HCl
6. customThe precipitate that formed
7. filtrationwas collected by filtration
8. washwashed with water and hexanes