反应详情

温度

120 °C

Methyl 3-(7-hydroxy-1-oxoisoquinolin-2(1H)-yl)-4-methylbenzoate (529 mg), N-phenyltrifluoromethanesulfonamide (612 mg) and potassium carbonate (709 mg) were stirred in THF (15 ml) and heated under microwave irradiation (Personal Chemistry Emrys Optimizer with 300 W magnetron) at 120° C. for 10 minutes. The reaction mixture was concentrated and the residue was dissolved in ethyl acetate and washed with water (×2), brine, dried (magnesium sulfate) and concentrated. Purification by column chromatography with a gradient of iso-hexane to 30% ethyl acetate/iso-hexane yielded methyl 4-methyl-3-[1-oxo-7-{[(trifluoromethyl)sulfonyl]oxy} isoquinolin-2(1H)-yl]benzoate as a white solid (613 mg); NMR Spectrum: (DMSOd6) 2.15 (s, 3H), 3.86 (s, 3H), 6.89 (d, 1H), 7.50 (d, 1H), 7.60 (d, 1H), 7.90 (s, 1H), 7.93 (d, 1H), 8.00 (m, 2H), 8.20 (s, 1H); Mass Spectrum: M+Na+ 464.

1. concentrationThe reaction mixture was concentrated
2. dissolutionthe residue was dissolved in ethyl acetate
3. washwashed with water (×2), brine
4. dry with materialdried (magnesium sulfate)
5. concentrationconcentrated
6. customPurification by column chromatography with a gradient of iso-hexane to 30% ethyl acetate/iso-hexane