반응 #46896

반응 방정식

5-chloro-2-trichloromethyl-1H-benzoimidazole

benzylamine

NaHCO3

→

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

용매

tetrahydrofuran

THF

water

반응 조건

후처리

1. 1
   여과The suspension was filtered
2. 2
   농축the filtrate was concentrated under reduced pressure
3. 3
   기타After purification by preparative RP-HPLC (CH3CN/H2O gradient and 0.05% formic acid) pure 5-Chloro-1H-benzoimidazole-2-carboxylic acid benzylamide
4. 4
   기타was obtained as a white amorphous solid

실험 절차

A solution of 120.0 mg (0.45 mmol) 5-chloro-2-trichloromethyl-1H-benzoimidazole in 2 mL tetrahydrofuran (THF) was added slowly to a mixture of 53.5 μl (0.49 mmol) benzylamine and 373.8 mg (4.45 mmol, 10 equiv.) NaHCO3 in 8 mL THF and 4 mL water. The reaction mixture was stirred for 2 h at room temperature (20° C. to 25° C. in the following RT). The suspension was filtered and the filtrate was concentrated under reduced pressure. After purification by preparative RP-HPLC (CH3CN/H2O gradient and 0.05% formic acid) pure 5-Chloro-1H-benzoimidazole-2-carboxylic acid benzylamide was obtained as a white amorphous solid.

출처