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

HRID 637891노트

반응식

HRID 637891 반응식
[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]

참가 물질

7

반응물 4

HCID 962WaterHCID 516951Monobasic potassium phosphateHCID 3032624Potassium nitrosodisulfonateHCID 20254624HCID 20254624, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 887Methanol용매HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-533294f5e54a4a9d98778a707d87cf80
출처 데이터셋
uspto-grants-1985_12
특허 번호
US04559177

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