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 was added a solution of 11.79 g (32.1 mmol) 2-trichloromethyl-1H-benzoimidazole-5-carboxylic acid methyl ester in 360 mL THF. The reaction mixture was stirred vigorously for 2 h at room temperature. The THF was evaporated. The precipitate was filtered off and treated twice with approx. 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 vacuo 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. Yield: 9.9 g

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