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Potassium Carbonate → HCID 67916683, Verbindung

HRID 846224
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 846224
Br[CH2:2][CH2:3][CH2:4][S:5][C:6]1[CH:11]=[CH:10][C:9]([C:12](=[O:21])[CH2:13][CH2:14][CH2:15][CH2:16][C:17]([O:19][CH3:20])=[O:18])=[CH:8][CH:7]=1.[CH3:22][CH2:23][CH2:24][C:25]1[C:30]([OH:31])=[C:29]([C:32]([CH3:34])=[O:33])[CH:28]=[CH:27][C:26]=1[OH:35].C(=O)([O-])[O-].[K+].[K+]>C(C(C)=O)C>[C:32]([C:29]1[CH:28]=[CH:27][C:26]([O:35][CH2:2][CH2:3][CH2:4][S:5][C:6]2[CH:11]=[CH:10][C:9]([C:12](=[O:21])[CH2:13][CH2:14][CH2:15][CH2:16][C:17]([O:19][CH3:20])=[O:18])=[CH:8][CH:7]=2)=[C:25]([CH2:24][CH2:23][CH3:22])[C:30]=1[OH:31])(=[O:33])[CH3:34]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 27751982',4'-Dihydroxy-3'-propylacetophenoneHCID 19884817HCID 19884817, Verbindung

Produkt 1

HCID 67916683HCID 67916683, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6569Methyl Ethyl KetoneLösungsmittel

Versuchsvorschrift

The compound of Step A above, (2.0 g, 5.36 mmoles), 2,4-dihydroxy-3-propylacetophenone (2.08 g, 10.72 mmole) and potassium carbonate (3.0 g, 21.44 mmole) were stirred in methyl ethyl ketone (100 ml) and heated at reflux for three hours. The reaction mixture was filtered and concentrated in vacuo. The residue was dissolved in ether-methanol and extracted with 1N NaOH (3×50 ml). The organics were dried and concentrated in vacuo. The residue was triturated with methanol, filtered and dried, to yield the title compound. NMR (CDCl3): 0.94 (3H, m), 1.73 (6H, m), 2.28 (6H, m), 2.95 (2H, m), 3.22 (2H, m), 3.66 (3H, s), 4.17 (2H, m), 6.42 (1H, d), 7.40 (2M, d), 7.61 (1H, d), 7.90 (2H, d), 12.73 (1H, s).

Aufarbeitung

  1. temperatureheated
  2. temperatureat reflux for three hours
  3. filtrationThe reaction mixture was filtered
  4. concentrationconcentrated in vacuo
  5. dissolutionThe residue was dissolved in ether-methanol
  6. extractionextracted with 1N NaOH (3×50 ml)
  7. customThe organics were dried
  8. concentrationconcentrated in vacuo
  9. customThe residue was triturated with methanol
  10. filtrationfiltered
  11. customdried

Quellen und Nachweise

ORD-Eintrag
ord-3b9eacfe17b343ed955f0e15fc33efca
Quelldatensatz
uspto-grants-1992_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05135940

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