反应详情

To a solution of (5-cyclopropyl-3-(2-trifluormethoxy-phenyl)-isoxazol-4-yl)-methanol (2.19 g, 7.32 mmol) in anhydrous methylene chloride (50 mL) at 0° C. is added PBr3 (0.83 mL, 8.7 mmol) and the mixture is stirred for 3 hours. The mixture is then poured into 100 mL of ice water and extracted with DCM (2×). The combined DCM layers are washed with brine, dried (MgSO4) and concentrated under reduced pressure to provide crude residue. The residue is purified via flash chromatography (120 g silica) eluting with a gradient of 0 to 60% ethyl acetate in heptane to provide the title compound (2.1 g, 79%) as an oil.

1. extractionextracted with DCM (2×)
2. washThe combined DCM layers are washed with brine
3. dry with materialdried (MgSO4)
4. concentrationconcentrated under reduced pressure
5. customto provide crude residue
6. customThe residue is purified via flash chromatography (120 g silica)
7. washeluting with a gradient of 0 to 60% ethyl acetate in heptane