反应详情

To a solution of tert-butyl(1-(4-(1-oxo-8-phenyl-2,4-dihydro-1H-pyrido[2,3-b][1,2,4]triazolo[4,3-d][1,4]oxazin-7-yl)phenyl)cyclobutyl)carbamate (26 mg, 0.05 mmol) in dry DMF (1 ml) was added potassium carbonate (21 mg, 0.15 mmol) and methyliodide (10 μl, 0.15 mmol) under nitrogen. The resulting mixture was stirred overnight at room temperature. Water was added and the mixture was extracted with EtOAc (3×5 ml). The combined organic phases were dried over Na2SO4 and concentrated to dryness under reduced pressure. The resulting residue was purified by Biotage silica gel chromatography (gradient 0 to 40% EtOAc in cyclohexane) to give the title compound (22 mg, 82%). 1H NMR (500 MHz, CDCl3): 8.50 (1H, s), 7.25 (2H, d), 7.20-7.19 (5H, m), 7.15-7.12 (2H, m), 5.21 (2H, s), 5.00 (1H, br s), 3.46 (3H, s), 2.55-2.25 (4H, m), 2.10-2.03 (1H, m), 1.86-1.78 (1H, m), 1.44-1.15 (9H, br).

1. extractionthe mixture was extracted with EtOAc (3×5 ml)
2. dry with materialThe combined organic phases were dried over Na2SO4
3. concentrationconcentrated to dryness under reduced pressure
4. customThe resulting residue was purified by Biotage silica gel chromatography (gradient 0 to 40% EtOAc in cyclohexane)