反应详情

A solution of 3-methylthiophene-2-carbaldehyde (10 g, 0.079 mol) in dichloromethane (10 ml) was added dropwise to a stirred solution of bromine (4.08 ml, 0.079 mol) in dichloromethane (15 ml) at room temperature. The resulting mixture was heated to reflux temperature for 3 hours before cooling to room temperature, washed with water (3×50 ml), saturated NaHCO3 solution (2×25 ml), dried (MgSO4) and the solvent removed at reduced pressure to give the sub-title compound as a brown solid (14.7 g, 66% yield): 1H NMR (400 MHz, CDCl3) δH 2.60 (3H, s), 6.97 (1H, s) 9.20 (1H, s).

1. temperatureThe resulting mixture was heated
2. temperatureto reflux temperature for 3 hours
3. washwashed with water (3×50 ml), saturated NaHCO3 solution (2×25 ml)
4. dry with materialdried (MgSO4)
5. customthe solvent removed at reduced pressure