反应详情

温度

80 °C

3-cyanophenol (2 000 mg; 16.79 mmol; 1 eq.) was dissolved in DMF (40 mL). Then ethyl 4-bromobutyrate (3 602.35 mg; 18.47 mmol; 1.10 eq.) and K2CO3 (3 480.55 mg; 25.18 mmol; 1.50 eq.) were added to the reaction mixture. The reaction mixture was heated to 80° C. for 2 hours. The reaction mixture was cooled to RT and diluted with EtOAc. The organic layer was washed with water (3×), brine, dried over MgSO4 and concentrated affording the title compound as a colourless liquid (3.92 g, 96%). 1H NMR (DMSO-d6, 300 MHz) δ 7.51-7.38 (m, 3H), 7.29-7.26 (m, 1H), 4.10-4.03 (m, 4H), 2.48-2.43 (t, J=7.37 Hz, 2H), 2.02-1.93 (m, 2H), 1.20-1.15 (t, J=7.10 Hz, 3H). HPLC (Method A) Rt 4.49 min (Purity: 97.9%).

1. temperatureThe reaction mixture was cooled to RT
2. washThe organic layer was washed with water (3×), brine
3. dry with materialdried over MgSO4
4. concentrationconcentrated