反应详情

A mixture of 1-(4-methoxyphenyl)-1H-benzimidazole-6-carbohydrazide (1.09 g, 3.86 mmol), potassium hydroxide (0.32 g, 5.79 mmol), carbon disulfide (2.31 mL, 38.6 mmol) and ethanol (20 mL) was stirred overnight at room temperature. The reaction mixture was concentrated under reduced pressure, N,N-dimethylformamide (15 ml) was added to the residue, and the resulting mixture was stirred at 100° C. overnight. The reaction mixture was acidified with 1M hydrochloric acid, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was washed with water to give the title compound (0.66 g, yield 53%) as colorless crystals.

1. concentrationThe reaction mixture was concentrated under reduced pressure, N,N-dimethylformamide (15 ml)
2. additionwas added to the residue
3. stirringthe resulting mixture was stirred at 100° C. overnight
4. extractionthe mixture was extracted with ethyl acetate
5. washThe organic layer was washed with saturated brine
6. dry with materialdried over anhydrous magnesium sulfate
7. concentrationconcentrated under reduced pressure
8. washThe residue was washed with water