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Ethyl-2-[2-(1,1-dimethylethyl)-4-oxo-4H-1-benzopyran-6-yl]propionate → Ethyl-2-[2,3-dihydro-2-(1,1-dimethylethyl)-4-oxo-4H-1-benzopyran-6-yl]propionate

HRID 26681
ノート
印刷プレビュー

反応式

HRID 26681 の反応式
[CH2:1]([O:3][C:4](=[O:22])[CH:5]([C:7]1[CH:8]=[CH:9][C:10]2[O:15][C:14]([C:16]([CH3:19])([CH3:18])[CH3:17])=[CH:13][C:12](=[O:20])[C:11]=2[CH:21]=1)[CH3:6])[CH3:2].CC(C)=O.OS(O)(=O)=O.O=[Cr](=O)=O>C(O)C.[Pd].CC(C)=O>[CH2:1]([O:3][C:4](=[O:22])[CH:5]([C:7]1[CH:8]=[CH:9][C:10]2[O:15][CH:14]([C:16]([CH3:18])([CH3:17])[CH3:19])[CH2:13][C:12](=[O:20])[C:11]=2[CH:21]=1)[CH3:6])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 54572468Ethyl-2-[2-(1,1-dimethylethyl)-4-oxo-4H-1-benzopyran-6-yl]propionateHCID 131709961Jones' reagent

生成物 1

HCID 54545077Ethyl-2-[2,3-dihydro-2-(1,1-dimethylethyl)-4-oxo-4H-1-benzopyran-6-yl]propionate

試薬・触媒・溶媒 3

HCID 23938Palladium触媒2 回HCID 180Acetone溶媒
HCID 702
Ethanol
溶媒

実験手順

Ethyl-2-[2-(1,1-dimethylethyl)-4-oxo-4H-1-benzopyran-6-yl]propionate (6.61 g) was taken up in dry ethanol (150 ml) and hydrogenated at 85 p.s.i. with 5% palladium on carbon (0.2 g) and 5% palladium on barium sulphate (0.4 g) for a total of 48 hours. The catalyst was removed by filtration (`Hyflo` supercel) and the ethanol removed in vacuo affording an oil. The oil was taken up in acetone (50 ml) and treated with a slight excess of Jones reagent. The excess oxidant was destroyed with methanol and the reaction mixture was dissolved in water (200 ml) and extracted with ether. The combined ethereal extracts were washed with water, dilute aqueous sodium bicarbonate solution and water, dried (MgSO4) and concentrated in vacuo to give the title compound as an oil - 6 g.

後処理

  1. customfor a total of 48 hours
  2. customThe catalyst was removed by filtration (`Hyflo` supercel) and the ethanol
  3. customremoved in vacuo
  4. customaffording an oil
  5. customThe excess oxidant was destroyed with methanol
  6. dissolutionthe reaction mixture was dissolved in water (200 ml)
  7. extractionextracted with ether
  8. washThe combined ethereal extracts were washed with water, dilute aqueous sodium bicarbonate solution and water
  9. dry with materialdried (MgSO4)
  10. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-ac8f4a81e1dd4b7caa6ee912ad10f7ca
出典データセット
uspto-grants-1979_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04151179

反応ノート

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