Water → 4-Ethylsulfonylbenzoic acid

HRID 271473

反応式

HRID 271473 の反応式
[CH2:1]([S:3][C:4]1[CH:12]=[CH:11][C:7]([C:8]([OH:10])=[O:9])=[CH:6][CH:5]=1)[CH3:2].S([O-])(O[O-])(=O)=[O:14].[K+].[K+].[OH2:21]>CO>[CH2:1]([S:3]([C:4]1[CH:12]=[CH:11][C:7]([C:8]([OH:10])=[O:9])=[CH:6][CH:5]=1)(=[O:14])=[O:21])[CH3:2]

参加物

5

反応物 3

HCID 962WaterHCID 832314-(Ethylthio)benzoic acidHCID 10313463Potassium peroxymonosulphate

生成物 1

HCID 1793674-Ethylsulfonylbenzoic acid

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a stirring solution of 4-(ethylthio)benzoic acid (1 g, 5.5 mmol) in methanol (30 mL) at 0° C. under argon was added a solution of potassium peroxymonosulfate (6.8 g, 11 mmol) in water (30 mL). The resulted suspension was stirred at room temperature for 15 h. Methanol was evaporated under vacuum, the reaction mixture was diluted with water (30 mL), and the product was extracted with EtOAc (2×30 mL). The combined organic phase was washed with saturated aqueous NaCl, dried (MgSO4), filtered and concentrated under reduced pressure to obtain 910 mg of title compound as a white solid. HPLC/MS: retention time=1.695 min, [M+H]+=215.

後処理

  1. customMethanol was evaporated under vacuum
  2. additionthe reaction mixture was diluted with water (30 mL)
  3. extractionthe product was extracted with EtOAc (2×30 mL)
  4. washThe combined organic phase was washed with saturated aqueous NaCl
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-b72705c2182d4eceafbc4e79c2daa821
出典データセット
uspto-grants-2008_11
特許番号
US07452892B2

関連ノート

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