反应详情

温度

60 °C

To a mixture of 4-hydroxy-1-(2-((1RS,2SR)-2-(2-hydroxypropan-2-yl)cyclopropyl)-1-methyl-1H-benzimidazol-6-yl)pyridin-2(1H)-one (100 mg), (4-chloro-3-fluorophenyl)methanol (0.073 ml), tributylphosphine (0.219 ml) and THF (10 ml) was added 1,1′-(azodicarbonyl)dipiperidine (223 mg), and the mixture was stirred at 60° C. overnight. The solvent was evaporated, and the residue was purified by column chromatography (hexane/EtOAc then EtOAc/MeOH), followed by NH silica gel column chromatography (hexane/EtOAc). The resulting solid was recrystallized from IPA-EtOAc to give the title compound (59.7 mg) as an off-white solid.

1. customThe solvent was evaporated
2. customthe residue was purified by column chromatography (hexane/EtOAc
3. customThe resulting solid was recrystallized from IPA-EtOAc