2',4'-Dihydroxyacetophenone → 7-Hydroxy-4-benzopyrone

HRID 333038

반응식

HRID 333038 반응식
[OH:1][C:2]1[CH:7]=[C:6]([OH:8])[CH:5]=[CH:4][C:3]=1[C:9](=[O:11])[CH3:10].[CH:12](OCC)(OCC)OCC.Cl(O)(=O)(=O)=O>CCOCC>[OH:8][C:6]1[CH:7]=[C:2]2[C:3]([C:9](=[O:11])[CH:10]=[CH:12][O:1]2)=[CH:4][CH:5]=1

참가 물질

5

반응물 3

HCID 69902',4'-DihydroxyacetophenoneHCID 24247Perchloric AcidHCID 31214Ethyl orthoformate

생성물 1

HCID 54092797-Hydroxy-4-benzopyrone수율 53.2%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

To a round bottomed flask, 0.26 mol of 2′,4′-dihydroxyacetophenone was added and mixed thoroughly with 232 mL of triethyl orthoformate. Then 26.4 mL of perchloric acid was dropped slowly into the resultant mixture. After 30 min reaction, 300 mL ether was added, and solids were precipitated. Following sucking filtration, the dried solids were transferred into a 1000 mL round bottomed flask, and refluxed for 2 hours after 250 mL hot water was added. Sucking filtration was conducted again, and then 22.69 g of 7-hydroxychromone was obtained by recrystallization with ethanol, with a yield of 53.2% and MS m/z (M)162.

후처리

  1. additionwas added
  2. customsolids were precipitated
  3. filtrationfiltration
  4. customthe dried solids were transferred into a 1000 mL round bottomed flask
  5. temperaturerefluxed for 2 hours after 250 mL hot water
  6. additionwas added
  7. filtrationSucking filtration

출처 및 근거

ORD 기록
ord-34c7645a78fd4fd8bd6cdfc84e744fcc
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08877949B2

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