反应详情

TEA (42 mg, 0.42 mmol), EDC.HCl (80 mg, 0.42 mmol), HOBt (57 mg, 0.418 mmol) and N-methyl-1-(4-(2-phenylpropan-2-yl)phenyl)methanamine (50 mg, 0.21 mmol) of Preparation 1 were sequentially added to a suspension of 8-hydroxyquinoline-7-carboxylic acid (48 mg, 0.25 mmol) in DCM (2.5 mL). The resulting reaction mixture was stirred at RT overnight. The mixture was quenched with H2O and then extracted three times with DCM. The separated organics were dried over Na2SO4, filtered and concentrated under reduced pressure. The residue was purified by flash chromatography (silica gel, DCM:MeOH 95:5) affording the title compound (39 mg, 0.1 mmol) as a grey solid. LC-MS m/z (ESI+): 411.2 (MH+), Rt=2.42 min (Method A).

1. customThe resulting reaction mixture
2. customThe mixture was quenched with H2O
3. extractionextracted three times with DCM
4. dry with materialThe separated organics were dried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customThe residue was purified by flash chromatography (silica gel, DCM:MeOH 95:5)