反应详情

温度

100 °C

A mixture of 2-chloro-3-hydroxypyridine (3.0 g, 23.1 mmol), β-bromophenetole (4.66 g, 23.2 mmol), and K2CO3 (8.0 g, 57.9 mmol) in DMF (50 mL) was heated at 100° C. for 1.5 h. The solvent was removed under reduced pressure and the residue was partitioned between EtOAc and H2O. The organic phase was dried (MgSO4), filtered, and the solvent evaporated. The solid residue was triturated with a small amount of ether and dried (65° C., 1 mmHg) to afford 4.23 g (74%) of the title product as white crystals: mp 77-78° C. Anal. (C13H12ClNO2) C, H, N.

1. customThe solvent was removed under reduced pressure
2. customthe residue was partitioned between EtOAc and H2O
3. dry with materialThe organic phase was dried (MgSO4)
4. filtrationfiltered
5. customthe solvent evaporated
6. customThe solid residue was triturated with a small amount of ether
7. customdried (65° C., 1 mmHg)