反应详情

1-Benzyl-4-[(N-ethylamino)methyl]piperidine (EXAMPLE 261, 5.68 g) and 2-chloro-3-nitropyridine (3.87 g) are dissolved in 96 ml of acetonitrile and 4.05 g of solid potassium bicarbonate is added. The reaction is refluxed for 20 hr, cooled to 20°-25°, poured into water and extracted with ethyl acetate. The organic extracts are dried (sodium sulfate), and concentrated under reduced pressure. Purification by flash column chromatography (15% ethyl acetate/hexane to 80% ethyl acetate/hexane) gives the title compound, HRMS calcd. for C20H26N4O2 =354.2056, found=354.2045.

1. temperatureThe reaction is refluxed for 20 hr
2. temperaturecooled to 20°-25°
3. extractionextracted with ethyl acetate
4. dry with materialThe organic extracts are dried (sodium sulfate)
5. concentrationconcentrated under reduced pressure
6. customPurification by flash column chromatography (15% ethyl acetate/hexane to 80% ethyl acetate/hexane)