Methylhydroquinone → 4-Hydroxy-3-methylphenyl acetate

HRID 131752

反応式

HRID 131752 の反応式
[C:1]([O:4][C:5](=[O:7])[CH3:6])(=O)[CH3:2].[OH:8][C:9]1[CH:14]=[CH:13]C(O)=[C:11](C)[CH:10]=1.C(=O)([O-])[O-].[Cs+].[Cs+]>C(#N)C>[C:5]([O:4][C:1]1[CH:11]=[CH:10][C:9]([OH:8])=[C:14]([CH3:13])[CH:2]=1)(=[O:7])[CH3:6]

参加物

5

反応物 3

HCID 7253MethylhydroquinoneHCID 7918Acetic AnhydrideHCID 10796Cesium carbonate

生成物 1

HCID 155324474-Hydroxy-3-methylphenyl acetate収率 3.1%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

Acetic anhydride (4.73 gm, 4.37 mL, 46.3 mMol) was added dropwise to a mixture of 4-hydroxy-2-methylphenol (5 gm, 46.3 mMol) and cesium carbonate (15.1 gm, 46.3 mMol) in acetonitrile (50 mL). After stirring overnight, the mixture was filtered and the filtrate was concentrated under reduced pressure. The residue was subjected to silica gel chromatography, eluting with 5:1 pentane:ethyl acetate. Fractions containing product were combined and concentrated under reduced pressure to provide 0.24 gm (3%) of the desired compound.

後処理

  1. filtrationthe mixture was filtered
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. washeluting with 5:1 pentane
  4. additionFractions containing product
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-9791b4f6a2c1460ebe7e3ef50b834101
出典データセット
uspto-grants-2008_06
特許番号
US07384983B2

関連ノート

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