Acetic Acid → HCID 20254624、化合物

HRID 2412839ノート

反応式

HRID 2412839 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.[H][H].[C:33](O)(=[O:35])[CH3:34]>[Pd]>[C:33]([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:35])[CH3:34]

参加物

6

反応物 4

HCID 176Acetic AcidHCID 24247Perchloric AcidHCID 132762366-(11-Hydroxy-1-oxoundecyl)-2,3-dimethoxy-5-methylphenolHCID 178418361HCID 178418361、化合物

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 of 6-(11-hydroxy-1-oxoundecyl)-2,3-dimethoxy-5-methylphenol (14 g) in acetic acid (200 ml) are added 5% palladium-on-carbon (50% hydrous) (3 g) and 70% perchloric acid (0.1 ml), and catalytic reduction is carried out at atmospheric temperature and pressure. When the hydrogen has ceased to be absorbed, 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 a 5% aqueous solution of sodium hydrogen carbonate and dried over anhydrous magnesium sulfate. The solvent is then distilled off to obtain a colorless oil of 6-(11-acetoxyundecyl)-2,3-dimethoxy-5-methylphenol (15 g).

後処理

  1. customto be absorbed
  2. filtrationthe catalyst is filtered off
  3. concentrationthe filtrate is concentrated under reduced pressure
  4. extractionThe residue is extracted with dichloromethane
  5. washthe dichloromethane layer is washed with a 5% aqueous solution of sodium hydrogen carbonate
  6. dry with materialdried over anhydrous magnesium sulfate
  7. distillationThe solvent is then distilled off

出典と根拠

ORDレコード
ord-d2e8c95e4ee44144a89b5834af3bb39c
出典データセット
uspto-grants-1985_01
特許番号
US04495104

反応ノート

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