Ethyl Acetate → 6-tert-butyl-8-fluoro-2-(2-hydroxymethyl-3-{1-methyl-6-oxo-5-[1'-(2,2,2-trifluoro-ethyl)-1',2',3',4',5',6'-hexahydro-[3,4']bipyridinyl-6-ylamino]-1,6-dihydro-pyridazin-3-yl}-phenyl)-2H-phthalazin-1-one

Participants

Reaction Steps

To a solution of 6-tert-butyl-8-fluoro-2-(2-(hydroxymethyl)-3-(1-methyl-6-oxo-5-(5-(piperidin-4-yl)pyridin-2-ylamino)-1,6-dihydropyridazin-3-yl)phenyl)phthalazin-1(2H)-one (10 mg, 16.4 μmol) in DMF (1 ml) was added potassium carbonate (6.8 mg, 49.2 μmol) and 2,2,2-trifluoroethyl trifluoromethanesulfonate (3.81 mg, 2.36 μl, 16.4 μmol) at room temperature. The mixture was stirred for 8 h. at the same temperature. EtOAc was added into the reaction mixture (10 mL) and the mixture was poured into water (10 mL). Organic layer was separated, washed with water (4×5 mL), dried (Na2SO4), and evaporated under vacuum. Crude product was purified by preparative tlc (CH2Cl2:MeOH:NH4OH, 90:9.5:0.5) to give 8 mg of pure product (70% yield): m/z 692[M+H]+.

Provenance & Evidence