反应详情

Into a 100 mL round bottom flask was placed (5-cyclopropyl-3-(2-(trifluoromethoxy)phenyl)isoxazol-4-yl)-methanol (4 g, 13.3 mmol), triphenylphosphine (5.6 g, 20 mmol, 1.5 equiv) and dichloromethane (40 mL). The mixture was stirred until completely dissolved, and then slowly cannulated dropwise into a stirring solution of carbon tetrabromide (6.6 g, 20 mmol, 1.5 eq) in dichloromethane (20 ml). The mixture was stirred for one hour and the solvent was then evaporated in vacuo. The crude residue was purified by silica gel chromatography using a 0-50% gradient of ethyl acetate/hexane. The desired product was obtained as a colorless oil. MS m/z 361.9/363.9 (M+1, Br79/Br81 isotope pattern).

1. customInto a 100 mL round bottom flask was placed
2. dissolutionuntil completely dissolved
3. stirringThe mixture was stirred for one hour
4. customthe solvent was then evaporated in vacuo
5. customThe crude residue was purified by silica gel chromatography