反应详情

温度

-20 °C

Saturated aqueous sodium hydrogencarbonate solution (375 ml) was added to a solution of 3-fluoro-4-(3-methyl-1,2,4-triazol-1-yl)phenylamine (Intermediate 27) (50.8 g, 0.265 mol) in THF (1 1). The mixture was cooled to −20° C. and benzyl chloroformate (48 ml, 0.336 mol) was added. The reaction mixture was stirred under N2, allowed to warm to room temperature and stirred for 2 days. The mixture was concentrated to approximately half the volume and diluted with ethyl acetate (1 l). The organic layer was separated and washed with water (2×), brine (2×), dried over sodium sulfate and concentrated in vacuo. Recrystallisation from ethyl acetate/hexanes (300 ml/200 ml) gave the title compound (73.0 g), m.p. 152.6-154.9° C.

1. temperatureto warm to room temperature
2. stirringstirred for 2 days
3. concentrationThe mixture was concentrated to approximately half the volume
4. additiondiluted with ethyl acetate (1 l)
5. customThe organic layer was separated
6. washwashed with water (2×), brine (2×)
7. dry with materialdried over sodium sulfate
8. concentrationconcentrated in vacuo
9. customRecrystallisation from ethyl acetate/hexanes (300 ml/200 ml)