反应详情

A mixture of 4-(bromomethyl)-3,5-dichloropyridine (15 g, 62.2 mmol), 4-hydroxybenzaldehyde (7.97 g, 65.4 mmol) and caesium carbonate (22.3 g, 68.5 mmol) in DMF (150 ml) was stirred for 4.5 h at room temperature. The mixture was poured into water and extracted with EtOAc. The organic extract was washed with sodium carbonate solution (×2) and brine, dried (MgSO4) and evaporated in vacuo to give the title compound as a brown solid (16 g). δH (DMSO-d6), 9.91 (1H, s), 8.74 (2H, s), 7.91 (2H, d, J 8.6 Hz), 7.27 (2H, d, J 8.6 Hz), 5.37 (2H, s); m/z (ESI) 282 (MH+).

1. extractionextracted with EtOAc
2. extractionThe organic extract
3. washwas washed with sodium carbonate solution (×2) and brine
4. dry with materialdried (MgSO4)
5. customevaporated in vacuo