反应详情

温度

25 °C

A mixture of 4-phenoxybenzoic acid (92 mg, 0.43 mmol), 1-hydroxybenzotriazole (80 mg, 0.6 mmol), 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (113 mg, 0.6 mmol), triethylamine (0.16 mL) and dichloromethane (15 mL) was stirred at 25° C. for half an hour. Then 5-(aminomethyl)-2,6-dimethylpyrimidin-4-ol (60 mg, 0.4 mmol) was added. The mixture was stirred at 25° C. for 12 hours and then concentrated to give a residue. The residue was purified by column chromatography (silica gel, dichloromethane/methanol=10:1) to give N-((4-hydroxy-2,6-dimethylpyrimidin-5-yl)methyl)-4-phenoxybenzamide as a white solid (30 mg, 21%). LRMS (M+H+) m/z: calcd 349.14. found 349. HPLC purity (214 nm): 98%. 1H NMR (300 MHz, d6-DMSO): δ 12.36 (s, 1H), 8.35 (t, J=4.5 Hz, 1H), 7.86 (d, J=8.4 Hz, 2H), 7.42 (t, J=8.4 Hz, 2H), 7.24-6.97 (m, 5H), 4.25 (d, J=4.5 Hz, 2H), 2.29 (s, 3H), 2.20 (s, 3H).

1. stirringThe mixture was stirred at 25° C. for 12 hours
2. concentrationconcentrated
3. customto give a residue
4. customThe residue was purified by column chromatography (silica gel, dichloromethane/methanol=10:1)