反应详情

温度

100 °C

A 250 ml three neck round bottom flask fitted with reflux condenser, pot thermometer and mechanical stirrer, was charged with 10 g (0.061 mol) of 2,6-dichlorophenol, 40 ml glacial acetic acid and 3.44 g (0.024 mol) of hexamethylenetetramine. The reaction mass was heated at reflux for 3 hrs (a clear solution was obtained at 70° C.). The progress of reaction was checked by TLC. The mixture was allowed to cool at 100° C.; 30 ml of 10% sulphuric acid were slowly added and stirred at 100° C. for 20-30 min. The reaction mass was poured into 200 g crushed ice. The solid was filtered and washed well with 100 ml water and drying at 70° C. afforded 9.2 g (84%) of 3,5-dichloro-4-hydroxy-benzaldehyde. Melting point: 153-155° C. 1H NMR (400 MHz, CD3OD) δ 9.72 (s, 1H), δ 7.80 (s, 1H).

1. temperaturewith reflux condenser
2. temperatureThe reaction mass was heated
3. temperatureat reflux for 3 hrs (a clear solution
4. customwas obtained at 70° C.)
5. customThe progress of reaction
6. additionThe reaction mass was poured into 200 g
7. customcrushed ice
8. filtrationThe solid was filtered
9. washwashed well with 100 ml water
10. customdrying at 70° C.