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