Water → 2-Bromo-4'-(methylsulfonyl)acetophenone

HRID 497172

反応式

HRID 497172 の反応式
[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

反応物 4

HCID 962WaterHCID 24408BromineHCID 825294-MethylsulfonylacetophenoneHCID 6451240Aluminum(III) Chloride

生成物 1

HCID 7358232-Bromo-4'-(methylsulfonyl)acetophenone収率 78%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

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

  1. extractionThe whole was extracted with ethyl acetate (50 mL×2)
  2. dry with materialthe combined organic layer was dried over MgSO4
  3. concentrationconcentrated in vacuo
  4. 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

関連ノート

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