Hydrochloric Acid → HCID 12832654、化合物

HRID 1903430ノート

反応式

HRID 1903430 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.Cl.C(=O)(O)[O-].[Na+]>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 313Hydrochloric AcidHCID 516892Sodium 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 (200 ml) of 6-(11-acetoxyundecyl)-2,3-dimethoxy-5-methyl-1,4-benzoquinone (4.2 g) in methanol is added concentrated hydrochloric acid (0.1 ml), and the mixture is allowed to stand at room temperature for 12 hours. To the reaction mixture is added sodium bicarbonate (0.2 g) and the solvent is distilled off. The product is dissolved in dichloromethane and the insoluble matter is filtered off. Removal of dichloromethane by distillation gives crude crystals. Recrystallization from hexane-ether (3:1) yields orange-yellow needles of 6-(11-hydroxyundecyl)-2,3-dimethoxy-5-methyl-1,4-benzoquinone (I, n=11) (3.6 g) m.p. 57° C.

後処理

  1. distillationthe solvent is distilled off
  2. dissolutionThe product is dissolved in dichloromethane
  3. filtrationthe insoluble matter is filtered off
  4. customRemoval of dichloromethane
  5. distillationby distillation
  6. customgives crude crystals
  7. customRecrystallization from hexane-ether (3:1)

出典と根拠

ORDレコード
ord-7ff19dfbb3b9447b8d1f941be238ccc2
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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