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Ozone → 2-(2-Oxoethyl)-7-methoxy-4-chromanone

HRID 264530
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 264530
[O:1]=[O+][O-].[CH2:4]([CH:8]1[CH2:17][C:16](=[O:18])[C:15]2[C:10](=[CH:11][C:12]([O:19][CH3:20])=[CH:13][CH:14]=2)[O:9]1)[CH:5]=CC>ClCCl.CO>[O:1]=[CH:5][CH2:4][CH:8]1[CH2:17][C:16](=[O:18])[C:15]2[C:10](=[CH:11][C:12]([O:19][CH3:20])=[CH:13][CH:14]=2)[O:9]1
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Komponenten

5

Edukt 2

HCID 24823Ozone2×HCID 54266277(RS)-2-(2-buten-1-yl)-7-methoxy-4-chromanone

Produkt 1

HCID 190365432-(2-Oxoethyl)-7-methoxy-4-chromanoneAusbeute 49 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

An ozone stream (3 g ozone/hour) was conducted while stirring for 1 hour through a solution, cooled to -70°, of 6.25 g of (RS)-2-(2-buten-1-yl)-7-methoxy-4-chromanone in 90 ml of anhydrous dichloromethane and 30 ml of anhydrous methanol. Subsequently, the solution was flushed with oxygen for 5 minutes and with argon for 15 minutes. After the addition of 3 ml of dimethyl sulfide, the mixture was stirred at room temperature for 16 hours. The reaction mixture was subsequently evaporated in a vacuum. The residue was treated with 60 ml of dichloromethane and, after the addition of 15 ml of water and 15 ml of trifluoroacetic acid, stirred at room temperature for 3 hours. The mixture was subsequently poured into 100 ml of water and neutralized while stirring by the spatula-wise addition of sodium hydrogen carbonate. An additional 70 ml of water were added. The phases were separated and the aqueous phase was extracted twice with 100 ml of dichloromethane each time. The combined organic phases were dried over magnesium sulfate and concentrated in a vacuum. 2.9 g (49%) of 2-(2-oxoethyl)-7-methoxy-4-chromanone were obtained as a yellow oil.

Aufarbeitung

  1. customSubsequently, the solution was flushed with oxygen for 5 minutes and with argon for 15 minutes
  2. additionAfter the addition of 3 ml of dimethyl sulfide
  3. stirringthe mixture was stirred at room temperature for 16 hours
  4. customThe reaction mixture was subsequently evaporated in a vacuum
  5. additionThe residue was treated with 60 ml of dichloromethane
  6. additionafter the addition of 15 ml of water and 15 ml of trifluoroacetic acid
  7. stirringstirred at room temperature for 3 hours
  8. additionThe mixture was subsequently poured into 100 ml of water
  9. stirringneutralized while stirring by the spatula-wise addition of sodium hydrogen carbonate
  10. additionAn additional 70 ml of water were added
  11. customThe phases were separated
  12. extractionthe aqueous phase was extracted twice with 100 ml of dichloromethane each time
  13. dry with materialThe combined organic phases were dried over magnesium sulfate
  14. concentrationconcentrated in a vacuum

Quellen und Nachweise

ORD-Eintrag
ord-e7ee94e7355947e9943c279b7a996a2a
Quelldatensatz
uspto-grants-1997_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05646173

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