反应详情

To a solution of 3-bromo-5-nitro-phenol (770 g, 3.53 mol) in acetone (10 L) was added pulverized K2CO3 (2.45 kg, 17.75 mol) in one portion at rt followed by addition of benzyl bromide (632 mL, 5.32 mol) over a period of 30 min. The resulting reaction mixture was stirred for 15 min then heated at reflux for 3 h. After reaction completion (by TLC), the reaction mixture was filtered through celite and the acetone distilled off. The crude residue thus obtained was purified over silica gel (60-120 M) using EtOAc:hexane (5:95) to obtain the desired product (551 g, 51%).

1. customat rt
2. customThe resulting reaction mixture
3. temperaturethen heated
4. temperatureat reflux for 3 h
5. customAfter reaction completion (by TLC)
6. filtrationthe reaction mixture was filtered through celite
7. distillationthe acetone distilled off
8. customThe crude residue thus obtained
9. customwas purified over silica gel (60-120 M)