反应详情

A solution of methyl 3-methyl-2-oxo-2,3-dihydro-1H-benzimidazole-4-carboxylate (500 mg, 2.42 mmol), N-chlorosuccinimide (355 mg, 2.66 mmol) and 2,2′-azobis(isobutyronitrile) (20 mg, 0.12 mmol) in carbon tetrachloride (40 mL) was refluxed for 2 days. After cooling, the reaction mixture was concentrated in vacuo. The resultant was extracted with ethyl acetate and water. The organics was dried over magnesium sulfate, filtered, and concentrated in vacuo. The residue was chromatographed on a silica gel to give 167 mg (0.07 mmol, 29%) of the title compound.

1. temperatureAfter cooling
2. concentrationthe reaction mixture was concentrated in vacuo
3. extractionThe resultant was extracted with ethyl acetate and water
4. dry with materialThe organics was dried over magnesium sulfate
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customThe residue was chromatographed on a silica gel