反应详情

温度

130 °C

Intermediate 36 (7.3 g, 30.6 mmol) was dissolved in DMF (70 mL). To this solution was added anhydrous K2CO3 (4.7 g, 33.7 mmol) and the mixture was heated to reflux (130° C.) for 5 h. The solvent was removed under pressure, the residue was poured into ice water, and the aq phase was extracted with EtOAc. The combined organic layers were dried over anhydrous Na2SO4, concentrated under vacuum, and the resulting yellow solid was recrystallized from EtOH to give 5-methoxy-1H-benzo[d]imidazol-2(3H)-one (intermediate 37) (3.6 g, 72%) as a yellow solid. mp: 249-251° C.

1. temperaturethe mixture was heated
2. customThe solvent was removed under pressure
3. additionthe residue was poured into ice water
4. extractionthe aq phase was extracted with EtOAc
5. dry with materialThe combined organic layers were dried over anhydrous Na2SO4
6. concentrationconcentrated under vacuum
7. customthe resulting yellow solid was recrystallized from EtOH