反应详情

To a solution of thiophene-3-carboxaldehyde (5.0 g, 44.58 mmole) in benzene (200 mL) was added ethylene glycol (25 mL, 445.8 mmole) and p-toluenesulfonic acid hydrate (848 mg, 4.458 mmole). The mixture was heated to reflux under a Dean-Stark trap. After 18 hr the mixture was cooled to RT, washed with saturated NaHCO3 then with H2O, dried (MgSO4), and concentrated under reduced pressure to give the title compound (6.32 g, 91%) as a light amber oil: 1H NMR (400 MHz, CDCl3) δ 7.42 (s, 1 H), 7.32 (m, 1 H), 7.16 (m, 1 H), 5.91 (s, 1 H), 4.12-3.99 (m, 4 H).

1. temperatureThe mixture was heated
2. temperatureto reflux under a Dean-Stark trap
3. washwashed with saturated NaHCO3
4. dry with materialwith H2O, dried (MgSO4)
5. concentrationconcentrated under reduced pressure