反应详情

温度

110 °C

To a solution of 2-(2,4-difluorophenyl)-4,5-dimethyl-2H-1,2,3-triazole 1-oxide (i.e. the product of Step A, 1.78 g, 7.0 mmol) in tetrahydrofuran (14 mL) was added trifluoroacetic anhydride (2.5 mL, 17.5 mmol). The reaction mixture was stirred at 110° C. in the microwave for 75 min. The mixture was diluted with ethyl acetate, washed successively with 1.0 M aqueous sodium hydroxide and 50% aqueous sodium hydroxide, dried (MgSO4) and concentrated under reduced pressure to afford the crude product. The crude material was purified by chromatography on silica gel eluting with 0 to 100% ethyl acetate in hexanes to obtain the title compound (0.59 g) as a colorless solid.

1. washwashed successively with 1.0 M aqueous sodium hydroxide and 50% aqueous sodium hydroxide
2. dry with materialdried (MgSO4)
3. concentrationconcentrated under reduced pressure
4. customto afford the crude product
5. customThe crude material was purified by chromatography on silica gel eluting with 0 to 100% ethyl acetate in hexanes