Water → 2-Bromo-4'-(methylsulfonyl)acetophenone
反応式
[CH3:1][C:2]([C:4]1[CH:9]=[CH:8][C:7]([S:10]([CH3:13])(=[O:12])=[O:11])=[CH:6][CH:5]=1)=[O:3].[Cl-].[Al+3].[Cl-].[Cl-].[Br:18]Br.O>C(Cl)(Cl)Cl>[Br:18][CH2:1][C:2]([C:4]1[CH:5]=[CH:6][C:7]([S:10]([CH3:13])(=[O:12])=[O:11])=[CH:8][CH:9]=1)=[O:3]参加物
6
実験手順
To a solution of 4-(methylsulfonyl)acetophenone (4.85 g, 24.5 mmol) in CHCl3 (70 ml) was added aluminum chloride (1 mg) and bromine (1.1 mL) in CHCl3 (8.5 mL) dropwise. The mixture was stirred overnight, and poured into water. The whole was extracted with ethyl acetate (50 mL×2), the combined organic layer was dried over MgSO4, and concentrated in vacuo. The resulting residue was recrystallized from ethyl acetate/hexane (1/1) to give the subtitle compound (5.28 g, 78% yield).
後処理
- extractionThe whole was extracted with ethyl acetate (50 mL×2)
- dry with materialthe combined organic layer was dried over MgSO4
- concentrationconcentrated in vacuo
- customThe resulting residue was recrystallized from ethyl acetate/hexane (1/1)
出典と根拠
- ORDレコード
- ord-14422ff21bb84ea78959e159be1bdf27
- 出典データセット
- uspto-grants-2005_09
- 特許番号
- US06949536B2
反応ノート
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