تفاعل #353263

ord-7c1c0db43bb942cfa734b09863dd1576

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 (23 g, 0.170 mmol) in carbon tetrachloride (80 mL). Add, by dropwise addition, a solution of bromine (26.85 g, 0.168 mmol) in carbon tetrachloride (30 mL) 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 (17.33 g, 48%); bp 64°-72° C. @0.02 mm Hg.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05650416uspto-grants-1997_07