Hydroxyamine hydrochloride → 6-Benzyloxy-2,2-dimethylchroman-4-one oxime

HRID 618817

Reaktionsgleichung

Reaktionsgleichung von HRID 618817
[CH2:1]([O:8][C:9]1[CH:10]=[C:11]2[C:16](=[CH:17][CH:18]=1)[O:15][C:14]([CH3:20])([CH3:19])[CH2:13][C:12]2=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.[NH2:23][OH:24]>C(O)C.N1C=CC=CC=1.CC(=O)OCC>[CH2:1]([O:8][C:9]1[CH:10]=[C:11]2[C:16](=[CH:17][CH:18]=1)[O:15][C:14]([CH3:20])([CH3:19])[CH2:13][C:12]2=[N:23][OH:24])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Komponenten

6

Edukt 2

HCID 443297Hydroxyamine hydrochlorideHCID 117809926-Benzyloxy-2,2-dimethylchroman-4-one

Produkt 1

HCID 867545186-Benzyloxy-2,2-dimethylchroman-4-one oxime

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 702EthanolLösungsmittelHCID 1049PyridineLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

By heating 11.3 g (40 mmol) of 6-benzyloxy-2,2-dimethylchroman-4-one with 3.1 g (44 mmol) of hydroxylamine hydrochloride in 27 ml of ethanol and 27 ml of pyridine for 3 h at 70° C., after distilling off the solvent in vacuo and precipitating with water, 12.5 g of product, m.p. 105-108° C., were obtained. The product was dissolved in EA, the solution was dried and concentrated, and the residue was crystallized using petroleum ether; m.p. 118-120° C.

Aufarbeitung

  1. distillationafter distilling off the solvent in vacuo
  2. customprecipitating with water, 12.5 g of product, m.p. 105-108° C.
  3. customwere obtained
  4. customthe solution was dried
  5. concentrationconcentrated
  6. customthe residue was crystallized

Quellen und Nachweise

ORD-Eintrag
ord-899e338ffebe49ea87a8eb780dc37a5a
Quelldatensatz
uspto-grants-1999_09
Patentnummer
US05955607

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