反应详情

温度

120 °C

Compound 61 (20 mg, 0.067 mmol) was suspended in dry dioxane (2 mL) with the sodium butoxide (13 mg, 0.13 mmol), dicyclohexyl-[2-(2,4,6-triisopropylphenyl)phenyl]phosphane (6 mg, 0.01 mmol), 4-bromo-1-methyl-pyridin-2-one (25 mg, 0.13 mmol) and tris-(dibenzylidineacetone)dipalladium(0) (6 mg, 0.007 mmol). The mixture was placed under N2 and heated in a microwave for 1 h at 120° C. The mixture was left at RT over 2 days. The mixture was transferred to a flask with MeOH and the solvent removed. The residue was suspended in 10% MeOH/DCM and applied to a silica column, eluting with EtOAc/heptane, followed by MeOH/DCM gradient, to afford Compound 134 (6.8 mg). 1H NMR (400 MHz, DMSO) δ 10.27 (s, 1H), 9.70 (s, 1H), 9.14 (s, 1H), 8.54 (s, 1H), 7.88 (s, 1H), 7.62 (d, J=7.5 Hz, 1H), 7.47-7.35 (m, 2H), 7.34-7.21 (m, 3H), 7.21-7.11 (m, 1H), 6.87 (d, J=2.3 Hz, 1H), 6.58 (dd, J=7.5, 2.4 Hz, 1H), 3.37 (s, 3H), 3.19-3.09 (m, 2H), 1.06 (t, J=7.2 Hz, 3H), [M+H]+ m/z=407.13.

1. customthe solvent removed
2. washeluting with EtOAc/heptane