反应 #8198

ord-891086c3a8cc43c7beb58f68c0a282e1

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度the resulting mixture is refluxed for two hours
  2. 2
    温度After cooling
  3. 3
    过滤the reaction mixture is filtered through a glass-fritted funnel
  4. 4
    浓缩the filtrate is concentrated
  5. 5
    其他The residue is triturated with petroleum ether and toluene

实验过程

3-Methylbenzo[b]thiophene (9.9 g, 67 mmol) is heated in carbon tetrachloride (133 ml ) to near reflux in the presence of n-bromosuccinimide (11.9 g, 67 mmol, 1.0 eq.). 2,2′Azobisisobutyronitrile (2.2 g, 13.3 mmol, 0.2 eq.) is added and the resulting mixture is refluxed for two hours. After cooling, the reaction mixture is filtered through a glass-fritted funnel, and the filtrate is concentrated. The residue is triturated with petroleum ether and toluene to afford 6.42 g of 3-Bromomethylbenzo[b]thiophene (42%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07087635B2uspto-grants-2006_08