反应详情

To a stirred solution of 2-tert-butyl-9-fluoro-3,6-dihydro-7H-benzo[h]imidazo[4,5-f]isoquinolin-7-one (40 mg, 0.129 mmol) in dry DMF (1.5 mL) at 0° C. was added NaH (60 wt. %) (6 mg, 0.15 mmol). After stirring for 5 minutes, iodomethane (9 μL, 0.142 mmol) was added, and the reaction mixture was slowly warmed to room temperature over 2 h. The mixture was cooled in ice bath and the reaction was quenched with water. The reaction mixture was diluted with EtOAc, washed with water followed by brine, then dried over Na2SO4. After removal of the solvent the crude was purified by preparative thin layer chromatography (1:9 MeOH:CH2Cl2 as eluent) to obtain the title compound as a mixture of imidazole tautomers.

1. temperatureThe mixture was cooled in ice bath
2. customthe reaction was quenched with water
3. additionThe reaction mixture was diluted with EtOAc
4. washwashed with water
5. dry with materialdried over Na2SO4
6. customAfter removal of the solvent the crude
7. customwas purified by preparative thin layer chromatography (1:9 MeOH:CH2Cl2 as eluent)