Nitric Acid → HCID 57742139、化合物

HRID 660323ノート

反応式

HRID 660323 の反応式
[CH2:1]([O:3][C:4](=[O:14])[CH:5]([C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([OH:13])[CH:8]=1)[CH3:6])[CH3:2].[N+:15]([O-])([OH:17])=[O:16].O>C(O)(=O)C>[CH2:1]([O:3][C:4](=[O:14])[CH:5]([C:7]1[CH:12]=[CH:11][C:10]([N+:15]([O-:17])=[O:16])=[C:9]([OH:13])[CH:8]=1)[CH3:6])[CH3:2]

参加物

5

実験手順

A solution of 2-(3-Hydroxy-phenyl)-propionic acid ethyl ester (19.0 g) in acetic acid (150 mL) was added nitric acid (11.3 g) at room temperature. The reaction mixture was stirred for 1 h at room temperature and added water. The mixture was extracted with EtOAc and the organic layer was dried over magnesium sulfate, filtered and concentrated in vacuo. The resulting residue was chromatographed on silica gel (n-Hex:EtOAc=10:1) to afford the product as yellow solid. (6.08 g, 26.0%)

後処理

  1. extractionThe mixture was extracted with EtOAc
  2. dry with materialthe organic layer was dried over magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customThe resulting residue was chromatographed on silica gel (n-Hex:EtOAc=10:1)

出典と根拠

ORDレコード
ord-006af1c787c4479ea159671ebdf48058
出典データセット
uspto-grants-2011_12
特許番号
US08084484B2

反応ノート

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