反应详情

A solution of 500.0 mg (1.85 mmol) 5-Chloro-2-trichloromethyl-1H-benzoimidazole in 20 mL THF was added slowly to a mixture of 286 μl (2.04 mmol) diisopropyl-amine and 1.55 g (18.5 mmol, 10 equivalents) NaHCO3 in 70 mL THF and 20 mL water. The reaction mixture was stirred for 2 h at RT. The organic solvent was evaporated. The formed crystalline material was filtered off and treated once with about 50 mL of a saturated NaHCO3-solution under ultrasonic conditions. The crystalline residue was filtered off again and washed twice with 20 mL water. Drying under reduced pressure at 35° C. gave pure 5-Chloro-1H-benzoimidazole-2-carboxylic acid diisopropylamide in form of a light brown crystalline solid.

1. customThe organic solvent was evaporated
2. filtrationThe formed crystalline material was filtered off
3. additiontreated once with about 50 mL of a saturated NaHCO3-solution under ultrasonic conditions
4. filtrationThe crystalline residue was filtered off again
5. washwashed twice with 20 mL water
6. customDrying under reduced pressure at 35° C.