反应详情

温度

117.5 °C

To 2,6-dibromopyridine (7.1 g, 30.0 mmol) was added NMP (16 ml), (3-fluorophenyl)methanamine (4.13 g, 33.0 mmol) and Huenig's Base (5.76 ml, 33.0 mmol) flushed with argon. The crude reaction mixture was stirred at 115-120° C. for 168 hr, followed by LCMS. The crude mixture was cooled, 250 ml of ethyl acetate was added, washed with saturated sodium bicarbonate (2×), water (2×), saturated salt solution (1×), dried sodium sulfate, filtered, concentrate. The crude was purified by silica gel chromatography using 120 g column, eluting from 0%-20% ethyl acetate with hexane. The desired fractions were concentrated to constant mass, giving 7.11 grams of the title compound as a free base used without further purification. LCMS (m/z): 281.1/283.1 (MH+), retention time=1.03 min.

1. customflushed with argon
2. customThe crude reaction mixture
3. washwashed with saturated sodium bicarbonate (2×), water (2×), saturated salt solution (1×), dried sodium sulfate
4. filtrationfiltered
5. concentrationconcentrate
6. customThe crude was purified by silica gel chromatography
7. washeluting from 0%-20% ethyl acetate with hexane
8. concentrationThe desired fractions were concentrated to constant mass