反应详情

温度

60 °C

A mixture of 3-(5-amino-3-tert-butyl-pyrazol-1-yl)-phenol (400 mg, 1.73 mmol), 3-chloropropanol (326 mg, 3.46 mmol), potassium carbonate (596 mg, 4.32 mmol) and sodium iodide (77 mg, 0.52 mmol) were combined in n-butanol (6 mL). The reaction mixture was heated at 60° C. for 4 days. The mixture was cooled to room temperature, water (100 mL) and EtOAc (100 mL) were added, and then the organic phase was washed with water and brine, dried (Na2SO4), and concentrated at reduced pressure. The residue was purified by MPLC (80:20 hexane/EtOAc) to give the product 3-[3-(5-amino-3-tert-butyl-pyrazol-1-yl)-phenoxy]-propan-1-ol (400 mg, 80%). 1H-NMR (DMSO-d6) δ 7.30 (t, 1H), 7.10 (m, 2H), 6.80 (d, 1H), 5.30 (s, 1H), 5.10 (bs, 2H), 4.0 (t, 2H), 3.60 (t, 3H), 1.80 (m, 2H), 1.30 (s, 9H); MS LC-MS [M+H]+=290.3, RT=1.05 min.

1. temperatureThe mixture was cooled to room temperature
2. washthe organic phase was washed with water and brine
3. dry with materialdried (Na2SO4)
4. concentrationconcentrated at reduced pressure
5. customThe residue was purified by MPLC (80:20 hexane/EtOAc)