Acetone → HCID 12355869, Verbindung

HRID 435844Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 435844
[OH:1][C:2]1[CH:17]=[CH:16][C:5]2[C:6](=[O:15])[CH:7]=[C:8]([C:10]([O:12][CH2:13][CH3:14])=[O:11])[O:9][C:4]=2[CH:3]=1.[C:18](=[O:21])([O-])[O-].[K+].[K+].[I-].[K+].[CH3:26][C:27]([CH3:29])=[O:28]>>[C:27]([C:29]1[CH:6]=[CH:7][C:8]([O:9][CH2:4][CH2:3][CH2:2][CH2:17][CH2:16][O:1][C:2]2[CH:17]=[CH:16][C:5]3[C:6](=[O:15])[CH:7]=[C:8]([C:10]([O:12][CH2:13][CH3:14])=[O:11])[O:9][C:4]=3[CH:3]=2)=[CH:10][C:18]=1[OH:21])(=[O:28])[CH3:26]

Komponenten

5

Edukt 4

HCID 180AcetoneHCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 5376802ethyl 7-hydroxy-4-oxo-4H-chromen-2-carboxylate

Produkt 1

HCID 12355869HCID 12355869, Verbindung

Versuchsvorschrift

A mixture of 3.05 parts of 4-(5-bromopentyloxy)-2-hydroxy acetophenone, 2.34 parts of ethyl 7-hydroxy-4-oxo-4H-1-benzopyran-2-carboxylate, 1.38 parts of potassium carbonate and 0.5 parts of potassium iodide, in 200 parts of dry acetone, was heated under reflux for 24 hours. The solution was filtered while hot and the inorganic salts washed with hot acetone. The solvent was removed to leave a yellow solid, which was washed with water and ether. The insoluble yellow solid was crystallised from ethyl alcohol to yield 3.3 parts of ethyl 7-[5-(4-acetyl-3-hydroxyphenoxy)pentyloxy]-4-oxo-4H-1-benzopyran-2-carboxylate as pale yellow needles, melting point 136°-137° C.

Aufarbeitung

  1. temperatureunder reflux for 24 hours
  2. filtrationThe solution was filtered while hot and the inorganic salts
  3. washwashed with hot acetone
  4. customThe solvent was removed
  5. customto leave a yellow solid, which
  6. washwas washed with water and ether
  7. customThe insoluble yellow solid was crystallised from ethyl alcohol

Quellen und Nachweise

ORD-Eintrag
ord-4b7444afa23f4ff8a37cb22991b90a32
Quelldatensatz
uspto-grants-1977_02
Patentnummer
US04006245

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