反应详情

温度

-78 °C

To a solution of 3-(2-fluoro-4-iodophenyl)-4-fluoro-8-methyl-1H-imidazo[4,5-g]quinazolin-2(3H)-one (example 34, step H) (90 mg, 0.22 mmol) in THF (5 ml) at −78° C. is added LiHMDS (0.29 ml, 1 M in THF, 0.29 mmol). The reaction mixture is stirred at −78° C. for 30 min and 1-(2-(tert-butyldimethylsilyloxy)ethyl)cyclopropane-1-sulfonyl chloride (99 mg, 0.33 mmol) is added to the mixture. The reaction is slowly warmed to room temperature and stirred at the temperature for 16 h. The reaction is quenched with saturated aqueous NH4Cl solution (20 ml) and extracted with EtOAc (2×30 ml). The combined organic solution is washed with brine (30 ml), dried over MgSO4 and concentrated. Silica gel chromatography yields the desired product.

1. temperatureThe reaction is slowly warmed to room temperature
2. stirringstirred at the temperature for 16 h
3. customThe reaction is quenched with saturated aqueous NH4Cl solution (20 ml)
4. extractionextracted with EtOAc (2×30 ml)
5. washThe combined organic solution is washed with brine (30 ml)
6. dry with materialdried over MgSO4
7. concentrationconcentrated