반응 #8198

ord-891086c3a8cc43c7beb58f68c0a282e1

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도the resulting mixture is refluxed for two hours
  2. 2
    온도After cooling
  3. 3
    여과the reaction mixture is filtered through a glass-fritted funnel
  4. 4
    농축the filtrate is concentrated
  5. 5
    기타The residue is triturated with petroleum ether and toluene

실험 절차

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%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07087635B2uspto-grants-2006_08