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Hydrochloric Acid → 4'-(Benzyloxy)-5-hydroxy-3,3',7-trimethoxyflavone

HRID 223125
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인쇄 미리보기

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HRID 223125 반응식
[OH:1][C:2]1[CH:7]=[C:6]([O:8][CH3:9])[CH:5]=[C:4]([OH:10])[C:3]=1[C:11](=[O:15])[CH2:12][O:13][CH3:14].[CH2:16]([O:23][C:24]1[CH:32]=[CH:31][C:27]([C:28]([O-])=O)=[CH:26][C:25]=1[O:33][CH3:34])[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.[Na+].[OH-].[K+].Cl>C(O)C.C(Cl)(Cl)Cl>[CH2:16]([O:23][C:24]1[CH:32]=[CH:31][C:27]([C:28]2[O:1][C:2]3[C:3]([C:11](=[O:15])[C:12]=2[O:13][CH3:14])=[C:4]([OH:10])[CH:5]=[C:6]([O:8][CH3:9])[CH:7]=3)=[CH:26][C:25]=1[O:33][CH3:34])[C:17]1[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 205225472',6'-Dihydroxy-2,4'-dimethoxyacetophenoneHCID 23702605Sodium 4-(benzyloxy)-3-methoxybenzoate

생성물 1

HCID 205225384'-(Benzyloxy)-5-hydroxy-3,3',7-trimethoxyflavone수율 62.7%

시약·촉매·용매 2

HCID 702
Ethanol
용매
HCID 6212Chloroform용매

실험 절차

A mixture of 0.67 g of 2',6'-dihydroxy-2,4'-dimethoxyacetophenone, 3.5 g of bis-[4-(benzyloxy)-3-methoxybenzoic] anhydride and 1 g of sodium 4-(benzyloxy)-3-methoxybenzoate was heated at 180°-185° C. under reduced pressure for 3 hours. After cooling, 12 ml of 10% solution of potassium hydroxide in ethanol were added, and the mixture was refluxed under nitrogen for 30 minutes. To the cooled mixture were added 20 ml of 1 N-hydrochloric acid and 100 ml of chloroform, followed by shaking. The organic phase was separated and concentrated under reduced pressure. The residue was chromatographed on silica gel with chloroform. After recrystallization from ethyl acetate/hexane, there was obtained 0.86 g (60% yield) of 4'-(benzyloxy)-5-hydroxy-3,3',7-trimethoxyflavone as yellow crystals: m.p. 156°-157° C.

후처리

  1. temperaturewas heated at 180°-185° C. under reduced pressure for 3 hours
  2. temperatureAfter cooling
  3. temperaturethe mixture was refluxed under nitrogen for 30 minutes
  4. customThe organic phase was separated
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was chromatographed on silica gel with chloroform
  7. customAfter recrystallization from ethyl acetate/hexane

출처 및 근거

ORD 기록
ord-cb01904e5f0d4d2db03f6503844c6b67
출처 데이터셋
uspto-grants-1982_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04352792

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