反应详情

The solution of 0.2 g (0.51 mmol) 2-[2-(4-chloro-phenyl)-5,6-difluoro-benzoimidazol-1-yl]-2-cyclohexyl-ethanol (Ex. 1, int. c) in 3 mL dichloromethane was cooled to 0° C. and 134 mg (0.51 mmol) triphenylphosphine and 170 mg (0.51 mmol) carbon tetrabromide were added. The reaction was stirred for 48 h at rt. and then evaporated. The residue was purified by silica gel chromatography using a MPLC system (CombiFlash Companion, Isco Inc.) eluting with a gradient of n-heptane:ethyl acetate (100:0 to 60:40) to give the desired compound as white solid (9%). MS (Turbo Spray): m/z=453.0 [M+H].

1. customand then evaporated
2. customThe residue was purified by silica gel chromatography
3. washeluting with a gradient of n-heptane:ethyl acetate (100:0 to 60:40)