Water → 6-(11-Acetoxyundecyl)-2,3-dimethoxy-5-methyl-1,4-benzoquinone

HRID 637891ノート

反応式

HRID 637891 の反応式
[C:1]([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]([OH:22])=[C:20]([O:23][CH3:24])[C:19]([O:25][CH3:26])=[CH:18][C:17]=1[CH3:27])(=[O:3])[CH3:2].N(S([O-])(=O)=O)(S([O-])(=O)=[O:31])[O].[K+].[K+].O.P(O)(O)([O-])=O.[K+]>CN(C)C=O.CO>[C:1]([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:31])[C:17]=1[CH3:27])(=[O:3])[CH3:2]

参加物

7

反応物 4

HCID 962WaterHCID 516951Monobasic potassium phosphateHCID 3032624Potassium nitrosodisulfonateHCID 20254624HCID 20254624、化合物

生成物 1

HCID 128326536-(11-Acetoxyundecyl)-2,3-dimethoxy-5-methyl-1,4-benzoquinone収率 77.2%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 6-(11-acetoxyundecyl)-2,3-dimethoxy-5-methylphenol (8 g) in dimethylformamide (400 ml) are added potassium nitrosodisulfonate (24 g), water (400 ml), methanol (30 ml) and monopotassium phosphate (1.0 g). The mixture is stirred at room temperature for 28 days. The reaction product is extracted with dichloromethane and the dichloromethane layer is washed with water and dried over magnesium sulfate. The solvent is distilled off to thereby leave crude crystals. The crude crystals are recrystallized from hexane to yield 6.4 g of 6-(11-acetoxyundecyl)-2,3-dimethoxy-5-methyl-1,4-benzoquinone as orange-yellow needles, m.p.: 41° C.

後処理

  1. extractionThe reaction product is extracted with dichloromethane
  2. washthe dichloromethane layer is washed with water
  3. dry with materialdried over magnesium sulfate
  4. distillationThe solvent is distilled off
  5. customto thereby leave crude crystals
  6. customThe crude crystals are recrystallized from hexane

出典と根拠

ORDレコード
ord-533294f5e54a4a9d98778a707d87cf80
出典データセット
uspto-grants-1985_12
特許番号
US04559177

反応ノート

読み込み中…