反应详情

In a 100 ml dry flask, (3-{[5-chloro-1-(4-fluorobutyl)-1H-benzimidazol-2-yl]methyl}-2-oxo-2,3-dihydro-1H-imidazo[4,5-c]pyridin-1-yl)acetic acid (P67, 300 mg, 0.69 mmol), diisopropylethylamine (0.29 mL, 2.08 mmol, 3 eq.), cyclopropylamine (60 μL, 0.83 mmol, 1.2 eq.) and 2-(1H-7-Azabenzotriazol-1-yl)-1,1,3,3-tetramethyl uronium hexafluorophosphate Methanaminium (HATU, 316.9 mg, 0.83 mmol, 1.2 eq.) were dissolved in DMF (50 mL). The solution was placed under N2 atmosphere and stirred at room temperature during 1 hour. The reaction mixture was diluted with water (20 ml) and extracted with dichloromethane (50 mL). The organic layer was dried with MgSO4 and evaporated. The residue was further crystallized in diisopropylether/acetonirile. The solid was filtered off and dried into the oven for 16 hours which gave 2-(3-{[5-chloro-1-(4-fluorobutyl)-1H-benzimidazol-2-yl]methyl}-2-oxo-2,3-dihydro-1H-imidazo[4,5-c]pyridin-1-yl)-N-cyclopropylacetamide (P68, 86 mg, 26%) as a white solid; LCMS m/z=471 (M+H)+

1. customIn a 100 ml dry flask
2. extractionextracted with dichloromethane (50 mL)
3. dry with materialThe organic layer was dried with MgSO4
4. customevaporated
5. customThe residue was further crystallized in diisopropylether/acetonirile
6. filtrationThe solid was filtered off
7. customdried into the oven for 16 hours which