Methylhydroquinone → 4-Hydroxy-3-methylphenyl acetate

HRID 131752

반응식

HRID 131752 반응식
[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]

참가 물질

5

반응물 3

HCID 7253MethylhydroquinoneHCID 7918Acetic AnhydrideHCID 10796Cesium carbonate

생성물 1

HCID 155324474-Hydroxy-3-methylphenyl acetate수율 3.1%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9791b4f6a2c1460ebe7e3ef50b834101
출처 데이터셋
uspto-grants-2008_06
특허 번호
US07384983B2

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