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Methanol → 4-Chloro-4'-methylsulfinylmethylbenzophenone

HRID 2100
ノート
印刷プレビュー

反応式

HRID 2100 の反応式
[Cl:1][C:2]1[CH:18]=[CH:17][C:5]([C:6]([C:8]2[CH:13]=[CH:12][C:11]([CH2:14][S:15][CH3:16])=[CH:10][CH:9]=2)=[O:7])=[CH:4][CH:3]=1.CO.I([O-])(=O)(=O)=[O:22].[Na+]>O>[Cl:1][C:2]1[CH:18]=[CH:17][C:5]([C:6]([C:8]2[CH:13]=[CH:12][C:11]([CH2:14][S:15]([CH3:16])=[O:22])=[CH:10][CH:9]=2)=[O:7])=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 887MethanolHCID 196893654-Chloro-4'-methylthiomethylbenzophenoneHCID 23667635Sodium periodate

生成物 1

HCID 187798984-Chloro-4'-methylsulfinylmethylbenzophenone収率 93%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

4-chloro-4'-methylthiomethylbenzophenone (4.2 g) was added to methanol (150 ml). Sodium periodate (3.6 g) dissolved in water (20 ml), was added to this solution, and the mixture was stirred for 16 hours at room temperature. The reaction mixture was concentrated, and water was added thereto. The mixture was extracted with ethyl acetate. The ethyl acetate layer was washed with water and then dried over anhydrous magnesium sulfate. Ethyl acetate was distilled off under reduced pressure. The residual solid was washed with n-hexane to obtain the desired product (4.1 g, melting point: 116° to 118° C., yield: 93%).

後処理

  1. additionwas added to this solution
  2. concentrationThe reaction mixture was concentrated
  3. additionwater was added
  4. extractionThe mixture was extracted with ethyl acetate
  5. washThe ethyl acetate layer was washed with water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. distillationEthyl acetate was distilled off under reduced pressure
  8. washThe residual solid was washed with n-hexane

出典と根拠

ORDレコード
ord-27d91eecd20e450da1b8e17f791b0eaa
出典データセット
uspto-grants-1998_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05728699

反応ノート

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