反応 #321882

反応方程式

benzo[b]thiophene

bromine

→

3-bromobenzo[b]thiophene

溶媒

carbon tetrachloride

carbon tetrachloride

反応条件

後処理

1. 1
   workup.ADDITIONAdd, by dropwise addition
2. 2
   その他Quench with a 1M solution of sodium thiosulfate
3. 3
   その他separate the organic phase
4. 4
   抽出Extract the aqueous phase with carbon tetrachloride
5. 5
   乾燥dry (MgSO4)
6. 6
   その他Evaporate the solvent in vacuo
7. 7
   workup.DISTILLATIONpurify by distillation

実験手順

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.

出典