反应详情

温度

60 °C

To a solution of 4-(1-Methyl-4-pyridin-4-yl-1H-pyrazol-3-yl)-phenol (50 mg) in dioxane (2 ml) was added triphenylphosphine (84 mg), quinoxaline-2-yl-methanol (48 mg) and di-t-butyl-aza-dicarboxylate (73 mg) and the reaction mixture was heated at 60° C. for 18 h. The reaction mixture was poured into 1N NaOH, extracted 3× methylene chloride, dried magnesium sulfate, filtered and concentration Purification via MPLC biotage chromatography provided the title compound (54 mg, 67%). 1H NMR (400 MHz, CDCl3) δ 9.09 (s, 1H), 8.45 (d, J=6.2 Hz, 2H), 8.10 (m, 2H), 7.77 (m, 2H), 7.55 (s, 1H), 7.37 (d, J=9.1 Hz, 2H), 7.10 (d, J=6.9 Hz, 2H), 7.01 (d, J=8.7, 2H), 5.41 (s, 2H), 3.94 (s, 3H); MS: (M+H m/z=394.4).

1. extractionextracted 3× methylene chloride, dried magnesium sulfate
2. filtrationfiltered
3. concentrationconcentration Purification via MPLC biotage chromatography