反应详情

A solution of 2-chloro-6-fluoroquinoline from Step D (0.8 g, 4.4 mmol) and piperazine (3.79 g, 44 mmol) in N,N-dimethylformamide (20 mL) is heated at 110° C. for 2 hours. The reaction is then basified with saturated aqueous sodium bicarbonate and extracted with ethyl acetate. The extracts are dried over anhydrous magnesium sulfate, filtered, and concentrated to give a tan oil. The oil is flash chromatographed on silica gel Merck-60 with a gradient of methanolic ammonia (5–10%) in ethyl acetate to provide the title compound (0.330 g) as an off-white solid, m.p. 110–111° C.

1. extractionextracted with ethyl acetate
2. dry with materialThe extracts are dried over anhydrous magnesium sulfate
3. filtrationfiltered
4. concentrationconcentrated
5. customto give a tan oil
6. customchromatographed on silica gel Merck-60 with a gradient of methanolic ammonia (5–10%) in ethyl acetate