Acetic Acid → 2-Methoxy-4-trifluoromethanesulfonyloxybenzoic acid

HRID 2243521ノート

反応式

HRID 2243521 の反応式
[CH3:1][O:2][C:3]1[CH:12]=[C:11]([O:13][S:14]([C:17]([F:20])([F:19])[F:18])(=[O:16])=[O:15])[CH:10]=[CH:9][C:4]=1[C:5]([O:7]C)=[O:6].S(=O)(=O)(O)O.C(O)(=O)C>O>[CH3:1][O:2][C:3]1[CH:12]=[C:11]([O:13][S:14]([C:17]([F:20])([F:18])[F:19])(=[O:16])=[O:15])[CH:10]=[CH:9][C:4]=1[C:5]([OH:7])=[O:6]

参加物

5

反応物 3

HCID 176Acetic AcidHCID 1118Sulfuric AcidHCID 23282575Methyl 2-methoxy-4-trifluoromethane-sulfonyloxybenzoate

生成物 1

HCID 231343522-Methoxy-4-trifluoromethanesulfonyloxybenzoic acid収率 37.5%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

A mixture of methyl 2-methoxy-4-trifluoromethane-sulfonyloxybenzoate (3.49 g), sulfuric acid (90%, 0.1 mL), acetic acid (10 mL) and water (2 mL) was heated under reflux for 16 hrs. The reaction mixture was diluted with water, and the mixture was extracted with ethyl acetate. The organic layer was washed with water and brine, and dried over an hydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The residue was purified by recrystallization (solvent: ethyl acetate/n-hexane) to afford the title compound (1.25 g).

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 16 hrs
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe organic layer was washed with water and brine
  5. dry with materialdried over an hydrous magnesium sulfate
  6. customThe solvent was evaporated under reduced pressure
  7. customThe residue was purified by recrystallization (solvent: ethyl acetate/n-hexane)

出典と根拠

ORDレコード
ord-aafc8c027b5b4da2b53de7266f47d3f5
出典データセット
uspto-grants-2010_03
特許番号
US07674938B2

反応ノート

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