反应详情

温度

0 °C

To a solution of 200 mg (0.512 mmol) 2-[2-(4-chloro-phenyl)-5,6-difluoro-benzoimidazol-1-yl]-2-cyclohexyl-ethanol (Ex. 1, int. c) in 5 ml tetrahydrofuran were added 126 mg (0.563 mmol) 2-(4-hydroxy-phenoxy)-2-methyl-propionic acid ethyl ester (CAS RN 42806-90-6) and 124 mg (0.614 mmol) tri-n-butylphosphin. The reaction mixture was cooled down to 0° C. 106 mg (0.614 mmol) N,N,N′,N′-tetramethylazodicarboxamide were added and the reaction mixture was stirred for 18 hours at room temperature. The reaction mixture was concentrated under vacuum and 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 70:30) to give the title compound as colorless solid (74%). MS (Turbo Spray): m/z=597.2 [M+H].

1. concentrationThe reaction mixture was concentrated under vacuum
2. customthe residue was purified by silica gel chromatography
3. washeluting with a gradient of n-heptane:ethyl acetate (100:0 to 70:30)