反应详情

A mixture of 1-(2-cyclopropyl-1-methyl-1H-benzo[d]imidazol-6-yl)-4-hydroxypyridin-2(1H)-one (400 mg), (5-fluorothiophen-2-yl)methanol (376 mg), tributylphosphine (1.07 ml), 1,1′-(azodicarbonyl)dipiperidine (1.08 g) and THF (40 ml) was stirred at 60° C. under a dry atmosphere (CaCl2 tube) for 3 h. After solvent was evaporated, the residue was purified by silica gel column chromatography (hexane/EtOAc then EtOAc/MeOH), followed by preparative HPLC (C18, mobile phase: H2O/CH3CN (0.1% TFA included)). The desired fraction was neutralized with saturated NaHCO3 solution, and extracted with EtOAc. The organic layer was separated, dried over MgSO4 and concentrated in vacuo to give the title compound (130 mg) as an off-white solid.

1. customAfter solvent was evaporated
2. customthe residue was purified by silica gel column chromatography (hexane/EtOAc
3. extractionextracted with EtOAc
4. customThe organic layer was separated
5. dry with materialdried over MgSO4
6. concentrationconcentrated in vacuo