تفاعل #321882

ord-ca2f65c1f4c94ef4be57b86f7d77fe73

المتفاعلات

الكواشف

لا شيء

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONAdd, by dropwise addition
  2. 2
    أخرىQuench with a 1M solution of sodium thiosulfate
  3. 3
    أخرىseparate the organic phase
  4. 4
    استخلاصExtract the aqueous phase with carbon tetrachloride
  5. 5
    تجفيفdry (MgSO4)
  6. 6
    أخرىEvaporate the solvent in vacuo
  7. 7
    workup.DISTILLATIONpurify by distillation

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05596003uspto-grants-1997_01