反应详情

A mixture of 1.213 g (5.0 mmol) of 2-chloro-5,6-dinitrobenzimidazole (22) and 1.398 g (25 mmol) of iron powder in 50 mL of AcOH was stirred at room temperature for 4 h. The reaction mixture was diluted with 100 mL of EtOAc, filtered, and the solid was washed with portions of EtOAc (total EtOAc used ~ 100 mL). The filtrate and washings were combined and washed with H2O (100 mL×3). The H2O layer was extracted with 100 mL of EtOAc. The EtOAc solutions were combined, evaporated, coevaporated with toluene (10 mL×3), MeOH (10 mL×2) to give a brown solid.

1. filtrationfiltered
2. washthe solid was washed with portions of EtOAc (total EtOAc used ~ 100 mL)
3. washwashed with H2O (100 mL×3)
4. extractionThe H2O layer was extracted with 100 mL of EtOAc
5. customevaporated
6. customto give a brown solid