Reaktion #46899

Reaktionsgleichung

5-Chloro-2-trichloromethyl-1H-benzoimidazole

diisopropyl-amine

NaHCO3

→

5-Chloro-1H-benzoimidazole-2-carboxylic acid diisopropylamide

Lösungsmittel

THF

THF

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe organic solvent was evaporated
2. 2
   FiltrationThe formed crystalline material was filtered off
3. 3
   workup.ADDITIONtreated once with about 50 mL of a saturated NaHCO3-solution under ultrasonic conditions
4. 4
   FiltrationThe crystalline residue was filtered off again
5. 5
   Waschenwashed twice with 20 mL water
6. 6
   SonstigeDrying under reduced pressure at 35° C.

Vorschrift

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.

Quelle