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Ethyl Acetate → HCID 22676901, Verbindung

HRID 1006314
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1006314
[CH2:1]([C:3]1[CH:12]=[CH:11][CH:10]2[CH:5]([C:6](=[O:16])[C:7]([C:13]([OH:15])=[O:14])=[CH:8][O:9]2)[CH:4]=1)[CH3:2].[CH2:17]([C:19]1[CH:20]=[C:21]2[C:26](=[CH:27][CH:28]=1)[O:25][CH:24]=[C:23](C=O)[C:22]2=[O:31])[CH3:18].[OH:32]OS([O-])=O.[K+].CCOC(C)=O>CN(C=O)C>[CH2:1]([C:3]1[CH:12]=[CH:11][CH:10]2[CH:5]([C:6](=[O:16])[C:7]([C:13]([OH:15])=[O:14])=[CH:8][O:9]2)[CH:4]=1)[CH3:2].[CH2:17]([C:19]1[CH:28]=[CH:27][CH:26]2[CH:21]([C:22](=[O:31])[C:23]([OH:32])=[CH:24][O:25]2)[CH:20]=1)[CH3:18]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 8857Ethyl AcetateHCID 27588496-Ethyl-3-formylchromoneHCID 22676903HCID 22676903, VerbindungHCID 23707502Potassium hydroxy sulfite

Produkt 2

HCID 22676901HCID 22676901, VerbindungHCID 22676903HCID 22676903, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel

1
HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

To prepare 6-ethyl-4-oxo-4a,8a-dihydro-4H-chromene-3-carboxylic acid, 6-ethyl-3-formyl chromone (0.25 g) was dissolved in DMF (10 mL), and OXONE (0.76 g) was added and stirred at room temperature for 3 hours with the reaction having a final volume (12 mL). The reaction was monitored by TLC or GC analysis. EtOAc was added to extract the products and 1N HCl was used to dissolve the salts. The organic extract was washed with 1N HCl (30 mL×3) and brine (30 mL), dried over Na2SO4, and the solvent was removed under reduced pressure to obtain 6-ethyl-4-oxo-4a,8a-dihydro-4H-chromene-3-carboxylic acid in 52% yield and 6-ethyl-3-hydroxy-4a,8a-dihydro-chromene-4-one in 34% yield after purification by silica gel column chromatography.

Aufarbeitung

  1. extractionto extract the products and 1N HCl
  2. dissolutionto dissolve the salts
  3. extractionThe organic extract
  4. washwas washed with 1N HCl (30 mL×3) and brine (30 mL)
  5. dry with materialdried over Na2SO4
  6. customthe solvent was removed under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-c16e355a8281464fab3f8c305bce874c
Quelldatensatz
uspto-grants-2004_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06787671B2

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