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Sodium Carbonate → 7-Methoxy-3,4-dihydro-1-benzoxepin-5-one oxime

HRID 1448062
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1448062
Cl.[NH2:2][OH:3].C(=O)([O-])[O-].[Na+].[Na+].[CH3:10][O:11][C:12]1[CH:13]=[CH:14][C:15]2[O:21][CH2:20][CH2:19][CH2:18][C:17](=O)[C:16]=2[CH:23]=1>O.C(O)C>[CH3:10][O:11][C:12]1[CH:13]=[CH:14][C:15]2[O:21][CH2:20][CH2:19][CH2:18][C:17](=[N:2][OH:3])[C:16]=2[CH:23]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 3

HCID 10340Sodium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 135224797-METHOXY-2,3,4,5-TETRAHYDRO-1-BENZOXEPIN-5-ONE

Produkt 1

HCID 858439917-Methoxy-3,4-dihydro-1-benzoxepin-5-one oxime

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittel
HCID 962
Water
Lösungsmittel
2×

Versuchsvorschrift

6.95 g of hydroxylamine hydrochloride dissolved in 15 ml of water and 5.3 g of sodium carbonate are added to a solution of 19.2 g of 7-methoxy-3,4-dihydro-1-benzoxepin-5-one in 45 ml of ethanol. The mixture is left at room temperature for 24 hours with stirring. 100 ml of water are then added and the alcohol is evaporated. The aqueous solution is make alkaline by the addition of soda and unreacted benzoxepin is extracted with ether. The aqueous phase is neutralised and the desired oxime is extracted with ether. After drying of the organic solution and evaporation of the solvent under reduced pressure, a white solid is obtained which, when recrystallised from cyclohexane yields 17 g of the desired pure product which has a melting point of 103° to 104° C.

Aufarbeitung

  1. customthe alcohol is evaporated
  2. additionby the addition of soda and unreacted benzoxepin
  3. extractionis extracted with ether
  4. extractionthe desired oxime is extracted with ether
  5. customAfter drying of the organic solution and evaporation of the solvent under reduced pressure
  6. customa white solid is obtained which, when
  7. customrecrystallised from cyclohexane
  8. customyields 17 g of the desired pure product which

Quellen und Nachweise

ORD-Eintrag
ord-9b4b12e384c74b5285ea963e701d317f
Quelldatensatz
uspto-grants-1979_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04179516

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