反应详情

NaH (60% in mineral oil) (21.8 mg, 0.544 mmol) is added to a solution of 1-(2-fluoro-4-iodophenyl)-5,7-dimethyl-1H-imidazo[4,5-c]pyridine-2,6(3H,5H)-dione (100 mg, 0.251 mmol) in dry DMF (5 mL) at 0° C. The cooling bath is removed and the solution stirred at room temperature for 1 hour. The solution is re-cooled to −5° C. in a dry-ice/acetone bath, and 1-[2-(tert-butyldimethylsilanyloxy)ethyl]-cyclopropanesulfonyl chloride (300 mg, 1 mmol) in dry THF (2 mL) is added. The mixture is warmed to room temperature and stirred for an additional 16 hours. The mixture is concentrated to give an oily residue and purified via flash chromatography (SiO2, EtOAc:MeOH=9:1) to give the title compound.

1. customThe cooling bath is removed
2. temperatureThe solution is re-cooled to −5° C. in a dry-ice/acetone bath
3. temperatureThe mixture is warmed to room temperature
4. stirringstirred for an additional 16 hours
5. concentrationThe mixture is concentrated
6. customto give an oily residue
7. custompurified via flash chromatography (SiO2, EtOAc:MeOH=9:1)