反应详情

温度

110 °C

To a solution of 2-chloro-6-methoxy-quinoline of Step C, (2.5 g, 12.91 mmol) in N,N-dimethylformamide (50 mL) is added piperazine (12 g) and the mixture is heated at 110° C. under nitrogen for 6 hours. The solution is diluted with saturated aqueous sodium bicarbonate and extracted with ethyl acetate. The extracts are dried over anhydrous magnesium sulfate and evaporated to dryness. The residue is flash chromatographed on silica gel Merck-60 using a gradient of methanol (4–10%) in dichloromethane containing 0.2% ammonium hydroxide to provide the title compound (1.6 g) as an off-white solid, m.p. 95–97° C.

1. extractionextracted with ethyl acetate
2. dry with materialThe extracts are dried over anhydrous magnesium sulfate
3. customevaporated to dryness
4. customchromatographed on silica gel Merck-60