反应详情

To a mixture of 7.53 g (35.3 mmol) 1-cyclopropyl-piperidin-4-ylamine dihydrochloride and 32.39 g (0.386 mol) NaHCO3 in 1300 mL THF and 370 mL water a solution of 11.79 g (32.1 mmol) 2-trichloromethyl-1H-benzoimidazole-5-carboxylic acid methyl ester in 360 mL THF was added. The reaction mixture was stirred vigorously for 2 h at RT. The THF was evaporated. The precipitate was filtered off and treated twice with about 300 mL of a saturated NaHCO3-solution under ultrasonic conditions. After filtration the resulting solid was washed twice with 150 mL water and dried under reduced pressure at 45° C. to give pure 2-(1-cyclopropyl-piperidin-4-ylcarbamoyl)-1H-benzoimidazole-5-carboxylic methyl ester in form of a light brown crystalline material.

1. additionwas added
2. customThe THF was evaporated
3. filtrationThe precipitate was filtered off
4. additiontreated twice with about 300 mL of a saturated NaHCO3-solution under ultrasonic conditions
5. filtrationAfter filtration the resulting solid
6. washwas washed twice with 150 mL water
7. customdried under reduced pressure at 45° C.