반응 #321882

ord-ca2f65c1f4c94ef4be57b86f7d77fe73

시약

없음

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONAdd, by dropwise addition
  2. 2
    기타Quench with a 1M solution of sodium thiosulfate
  3. 3
    기타separate the organic phase
  4. 4
    추출Extract the aqueous phase with carbon tetrachloride
  5. 5
    건조dry (MgSO4)
  6. 6
    기타Evaporate the solvent in vacuo
  7. 7
    workup.DISTILLATIONpurify by distillation

실험 절차

Dissolve benzo[b]thiophene (23g, 0.170mmol) in carbon tetrachloride (80mL). Add, by dropwise addition, a solution of bromine (26.85g, 0.168mmol) in carbon tetrachloride (30mL) and stir at room temperature for 2 days. Quench with a 1M solution of sodium thiosulfate and separate the organic phase. Extract the aqueous phase with carbon tetrachloride, combine the organic phases and dry (MgSO4). Evaporate the solvent in vacuo and purify by distillation to give 3-bromobenzo[b]thiophene as a pale yellow liquid (17.33g, 48%); bp 64°-72° C.@0.02mm Hg.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05596003uspto-grants-1997_01