反应详情

To a solution of 2-methyl-2-((5-(trifluoromethyl)pyridin-2-yl)oxy)propanoic acid (0.204 g, 0.81 mmol) in dry DMF (6 mL) was added TBTU (0.289 g, 0.90 mmol) at room temperature under atmosphere of nitrogen. To this 4-(4-fluoro-3-(piperazine-1-carbonyl)benzyl)phthalazin-1(2H)-one (0.3 g, 0.81 mmol) and DIPEA (0.303 mL, 1.74 mmol) were added. The reaction mixture was stirred at room temperature for 2 h. The progress of reaction was checked by TLC by using mobile phase 5% methanol in chloroform. The reaction mixture was diluted with ethyl acetate. The organic layer was washed with water, dried over anhydrous Na2SO4 and solvents were evaporated on a rotatory evaporator under reduced pressure to crude solid which was purified by the flash column chromatography using eluent chloroform:methanol (98.3:1.7) to afford 4-(4-fluoro-3-(4-(2-methyl-2-((5-(trifluoromethyl)pyridin-2-yl)oxy)propanoyl)piperazine-1-carbonyl)benzyl)phthalazin-1(2H)-one as white solid (0.230 g, 47%).

1. customThe progress of reaction
2. washThe organic layer was washed with water
3. dry with materialdried over anhydrous Na2SO4 and solvents
4. customwere evaporated on a rotatory evaporator under reduced pressure to crude solid which
5. customwas purified by the flash column chromatography