Ethanol → HCID 12824119、化合物

HRID 1390586ノート

反応式

HRID 1390586 の反応式
[CH3:1][C:2]1[C:3](=[O:19])[C:4]([CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][C:16]([OH:18])=[O:17])=[C:5]([CH3:10])[C:6](=[O:9])[C:7]=1[CH3:8].O.[CH2:21](O)[CH3:22]>S(=O)(=O)(O)O>[CH3:1][C:2]1[C:3](=[O:19])[C:4]([CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][C:16]([O:18][CH2:21][CH3:22])=[O:17])=[C:5]([CH3:10])[C:6](=[O:9])[C:7]=1[CH3:8]

参加物

5

反応物 3

HCID 702EthanolHCID 962WaterHCID 129061502,3,5-Trimethyl-6-(5'-carboxypentyl)-1,4-benzoquinone

生成物 1

HCID 12824119HCID 12824119、化合物

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid触媒

実験手順

To a well stirred solution of 2,3,5-trimethyl-6-(5'-carboxypentyl)-1,4-benzoquinone (formula I-2 wherein R=H3C, n=4, in the free form) (0.21 part) in ethanol (10 volume parts) was added 3 drops of concentrated sulfuric acid under cooling in ice bath and kept standing for 12 hours. After addition of water, the reaction mixture was extracted with diethyl ether and the diethylether layer was washed with water and dried over anhydrous sodium sulfate. The residue upon removal of the solvent was subjected to chromatography on silica gel and eluted with chloroform to give 2,3,5-trimethyl-6-(5'-ethoxycarbonylpentyl)-1,4-benzoquinone (formula I-2 wherein R=H3C, n=4, in the form of ethyl ester) (0.20 part) as an orange oil.

後処理

  1. temperatureunder cooling in ice bath
  2. extractionthe reaction mixture was extracted with diethyl ether
  3. washthe diethylether layer was washed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe residue upon removal of the solvent
  6. washeluted with chloroform

出典と根拠

ORDレコード
ord-86557230a8ca4c0f99afdf2f372ac48c
出典データセット
uspto-grants-1979_02
特許番号
US04139545

反応ノート

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