反应详情

温度

110 °C

To a solution of [5-ethoxy-2-(4-fluorophenyl)-2H-1,2,3-triazol-4-yl][2-(trifluoromethyl)-4-pyridinyl]methanone (i.e. the product of Step C, 2.7 g, 7.1 mmol) in acetic acid (15 mL) was added iodine (1.8 g, 7.1 mmol) and hypophosphorous acid (50% in water, 3.1 mL, 28.4 mmol). The mixture was heated to 110° C. under a nitrogen atmosphere for 6 h. The reaction mixture was cooled to 23° C. and neutralized to ˜pH 7 with 1 M NaOH and a saturated aqueous sodium bicarbonate solution. The mixture was extracted with ethyl acetate (2×15 mL), dried (MgSO4) and concentrated under reduced pressure. The crude residue was purified by chromatography on silica gel eluting with 0 to 20% ethyl acetate in hexanes to afford the title compound (2.1 g) as an off-white solid.

1. temperatureThe reaction mixture was cooled to 23° C.
2. extractionThe mixture was extracted with ethyl acetate (2×15 mL)
3. dry with materialdried (MgSO4)
4. concentrationconcentrated under reduced pressure
5. customThe crude residue was purified by chromatography on silica gel eluting with 0 to 20% ethyl acetate in hexanes