Sulfuric Acid → HCID 12832654、化合物

HRID 637892ノート

反応式

HRID 637892 の反応式
C([O:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][C:16]1[C:21](=[O:22])[C:20]([O:23][CH3:24])=[C:19]([O:25][CH3:26])[C:18](=[O:27])[C:17]=1[CH3:28])(=O)C.S(=O)(=O)(O)O.C(=O)([O-])O.[K+]>CO>[OH:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][C:16]1[C:21](=[O:22])[C:20]([O:23][CH3:24])=[C:19]([O:25][CH3:26])[C:18](=[O:27])[C:17]=1[CH3:28]

参加物

5

反応物 3

HCID 1118Sulfuric AcidHCID 516893Potassium BicarbonateHCID 128326536-(11-Acetoxyundecyl)-2,3-dimethoxy-5-methyl-1,4-benzoquinone

生成物 1

HCID 12832654HCID 12832654、化合物収率 95.9%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of 6-(11-acetoxyundecyl)-2,3-dimethoxy-5-methyl-1,4-benzoquinone (4.2 g) in methanol (200 ml) is added concentrated sulfuric acid (0.1 ml) and the mixture is kept standing at room temperature for 12 hours. To a reaction mixture is added potassium hydrogencarbonate (0.2 g) and the solvent is distilled off. The resultant is dissolved in dichloromethane and insolubles are filtered off. Dichloromethane is distilled off to leave crude crystals. Recrystallization from hexane-ether (3:1) gives 6-(11-hydroxyundecyl)-2,3-dimethoxy-5-methyl-1,4-benzoquinone (3.6 g) as orange-yellow needles. m.p.: 57° C.

後処理

  1. distillationthe solvent is distilled off
  2. dissolutionThe resultant is dissolved in dichloromethane
  3. filtrationinsolubles are filtered off
  4. distillationDichloromethane is distilled off
  5. customto leave crude crystals
  6. customRecrystallization from hexane-ether (3:1)

出典と根拠

ORDレコード
ord-28170f8417d442e9b2372b0cf717d020
出典データセット
uspto-grants-1985_12
特許番号
US04559177

反応ノート

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