反应详情

6.2 Grams of a 2-Cyanobenzimidazole compound [compound (iv)]]of the formula (II) in which X is H and Z is OCF2O was dissolved in 100 ml of acetonitrile. 10 Grams of potassium carbonate was added thereto. The resulting mixture was heated under reflux for 15 minutes. Thereafter, 6.7 g of dimethylsulfamoyl chloride was added thereto. Refluxing was continued for 15 minutes with heating. The reaction solution was poured into ice water and extracted with ethyl acetate. The organic layer was washed with water and dried over anhydrous sodium sulfate. Crystals were obtained by removing the solvent from the dried layer by distillation. Recrystallizing the crystals from hexane/ethyl acetate and then from chloroform/methanol gave 2.4 g of benzimidazole derivative [present compound (15)]of the formula (I) in which X is H, Z is OCF2O, R is CN and Q is N(CH3)2.

1. temperatureThe resulting mixture was heated
2. temperatureunder reflux for 15 minutes
3. temperatureRefluxing
4. temperaturewith heating
5. extractionextracted with ethyl acetate
6. washThe organic layer was washed with water
7. dry with materialdried over anhydrous sodium sulfate
8. customCrystals were obtained
9. customby removing the solvent from the dried layer
10. distillationby distillation
11. customRecrystallizing the crystals from hexane/ethyl acetate