反应详情

温度

130 °C

CoppeeI cyanide (39.3 g, 0.44 mol, 1.2 eq) is added at room temperature to a stirred solution of 8-bromo-7-chloro-2-methoxy-[1,5]naphthyridine (100 g, 0.37 mol, 1.0 eq) in N,N-dimethylformamide (1.5 L). After 8 hours stirring at 130° C., the reaction mixture is cooled down to room temperature and treated with a saturated ammonium chloride aqueous solution (1.5 L). The aqueous layer is separated and extracted with ethyl acetate (2×1.5 L). The combined organic layers are dried over sodium sulfate, filtered and concentrated to give a residue that is washed with ethanol (20 mL) to afford 3-chloro-6-methoxy-[1,5]naphthyridine-4-carbonitrile as an off-white solid (49.5 g, 62% yield).

1. temperaturethe reaction mixture is cooled down to room temperature
2. customThe aqueous layer is separated
3. extractionextracted with ethyl acetate (2×1.5 L)
4. dry with materialThe combined organic layers are dried over sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated
7. customto give a residue that
8. washis washed with ethanol (20 mL)