反应详情

温度

100 °C

2-Fluorobenzonitrile (15.7 mL, 149 mmol) and 4-(methylsulfanyl)phenol (25 g, 178 mmol) were dissolved in DMF (500 mL) and K2CO3 (61.8 g, 447 mmol) was then added. The mixture was heated at 100° C. for 16 h under a nitrogen atmosphere. After cooling to room temperature the mixture was evaporated to dryness and then partitioned between ether (1 L) and water (2 L). The organic layer was separated, washed with 2M NaOH (500 mL), 10% (aq) K2CO3 (500 mL), dried (MgSO4) and evaporated to give a light brown solid (35.62 g, 92%); δH (CDCl3, 400 MHz) 2.50 (3H, s), 6.82 (1H, d), 7.05 (2H, d), 7.15 (1H, t), 7.30 (2H, m), 7.43 (1H, t), 7.62 (1H, d); MS m/z (TS+) 259 (MNH4+).

1. temperatureAfter cooling to room temperature the mixture
2. customwas evaporated to dryness
3. custompartitioned between ether (1 L) and water (2 L)
4. customThe organic layer was separated
5. washwashed with 2M NaOH (500 mL), 10% (aq) K2CO3 (500 mL)
6. dry with materialdried (MgSO4)
7. customevaporated