Acetic Acid → HCID 20254624、化合物

HRID 1903428ノート

反応式

HRID 1903428 の反応式
[OH:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][C:12]([C:14]1[C:19]([OH:20])=[C:18]([O:21][CH3:22])[C:17]([O:23][CH3:24])=[CH:16][C:15]=1[CH3:25])=O.Cl(O)(=O)(=O)=O.[C:31](O)(=[O:33])[CH3:32]>[Pd]>[C:31]([O:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][C:14]1[C:19]([OH:20])=[C:18]([O:21][CH3:22])[C:17]([O:23][CH3:24])=[CH:16][C:15]=1[CH3:25])(=[O:33])[CH3:32]

参加物

5

反応物 3

HCID 176Acetic AcidHCID 24247Perchloric AcidHCID 132762366-(11-Hydroxy-1-oxoundecyl)-2,3-dimethoxy-5-methylphenol

生成物 1

HCID 20254624HCID 20254624、化合物

試薬・触媒・溶媒 1

HCID 23938Palladium触媒

実験手順

To a solution (200 ml) of 6-(11-hydroxy-1-oxoundecyl)-2,3-dimethoxy-5-methylphenol (14 g) in acetic acid is added 5% palladium-on-carbon (50% hydrate; 3 g) and 70% perchloric acid (0.1 ml), and catalytic reduction is carried out at ambient temperature and atmospheric pressure. After completion of the absorption of hydrogen, the catalyst is filtered off and the filtrate is concentrated under reduced pressure. The residue is extracted with dichloromethane, and the dichloromethane layer is washed with 5% aqueous sodium bicarbonate and dried over anhydrous sodium sulfate. Removal of the solvent by distillation gives a colorless oil of 6-(11-acetoxyundecyl)-2,3-dimethoxy-5-methylphenol (15 g).

後処理

  1. customis carried out at ambient temperature
  2. customAfter completion of the absorption of hydrogen
  3. filtrationthe catalyst is filtered off
  4. concentrationthe filtrate is concentrated under reduced pressure
  5. extractionThe residue is extracted with dichloromethane
  6. washthe dichloromethane layer is washed with 5% aqueous sodium bicarbonate
  7. dry with materialdried over anhydrous sodium sulfate
  8. customRemoval of the solvent
  9. distillationby distillation

出典と根拠

ORDレコード
ord-8e22dc1fdd89451b8dd7bc60f505aebb
出典データセット
uspto-grants-1984_03
特許番号
US04436753

反応ノート

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