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

HRID 1903429노트

반응식

HRID 1903429 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 (400 ml) of 6-(11-acetoxyundecyl)-2,3-dimethoxy-5-methylphenol (8 g) in dimethylformamide are added potassium nitrosodisulfonate (24 g), water (400 ml), methanol (30 ml) and potassium dihydrogen phosphate (1.0 g), and the mixture is stirred at room temperature for 28 days. The product is extracted with dichloromethane and the dichloromethane layer is washed with water and then dried over anhydrous magnesium sulfate. Removal of the solvent by distillation gives crude crystals. Recrystallization from hexane yields orange-yellow needles of 6.4 g of 6-(11-acetoxyundecyl)-2,3-dimethoxy-5-methyl-1,4-benzoquinone. m.p. 41° C.

후처리

  1. extractionThe product is extracted with dichloromethane
  2. washthe dichloromethane layer is washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customRemoval of the solvent
  5. distillationby distillation
  6. customgives crude crystals
  7. customRecrystallization from hexane

출처 및 근거

ORD 기록
ord-370c4f83c4524ae090c5c4a2fe360aae
출처 데이터셋
uspto-grants-1984_03
특허 번호
US04436753

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