反应详情

Sodium hydride (60% in mineral oil) (234 mg, 5.86 mmol) was added portionwise to a solution of 5-(3-fluorophenyl)-1,3-dimethyl-1H-pyrrolo[3,4-d]pyrimidine-2,4(3H,6H)-dione (Intermediate Nf) (1000 mg, 3.66 mmol) and dibenzo-18-crown-6 (132 mg, 0.366 mmol) in DMF (28.1 mL) at 0° C. The solution was warmed to room temperature and stirred for 20 minutes, then re-cooled to 0° C. (2,2-Dimethyl-1,3-dioxolan-4-yl)methyltrifluoromethane sulfonate (Intermediate Sb) (1547 mg, 5.86 mmol) was added dropwise over 5 minutes. The mixture was warmed to room temperature and stirred for 3 hours. The reaction was quenched with saturated NH4Cl(aq) (10 mL) and extracted with DCM (3×30 mL). The combined organic extracts were dried over magnesium sulfate and evaporated under vacuum to afford the title compound as a red/brown amorphous solid.

1. additionwas added dropwise over 5 minutes
2. temperatureThe mixture was warmed to room temperature
3. stirringstirred for 3 hours
4. customThe reaction was quenched with saturated NH4Cl(aq) (10 mL)
5. extractionextracted with DCM (3×30 mL)
6. dry with materialThe combined organic extracts were dried over magnesium sulfate
7. customevaporated under vacuum