Sulfuric Acid → HCID 12832654, 화합물

HRID 637892노트

반응식

HRID 637892 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

HCID 12832654HCID 12832654, 화합물수율 95.9%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-28170f8417d442e9b2372b0cf717d020
출처 데이터셋
uspto-grants-1985_12
특허 번호
US04559177

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