Reaktion #60356

ord-5251abb8ef3d4e07a721a91e6cc405c5

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe mixture was heated
  2. 2
    Temperaturto reflux for 2 h
  3. 3
    Einengenconcentrated in vacuo
  4. 4
    Filtrationfiltered
  5. 5
    WaschenThe pad was washed with H2O (2×50 mL) and Et2O (2×50 mL)
  6. 6
    Sonstigethe solids were dried in vacuo

Vorschrift

To a mixture of 6-bromo-3,4-dihydro-1H-naphthalen-2-one (5.370 g, 23.86 mmol) and hydroxylamine hydrochloride (2.487 g, 35.79 mmol) in EtOH (80 mL) was added a solution of NaOAc (5.871 g, 71.57 mmol) in H2O (20 mL). The mixture was heated to reflux for 2 h. The reaction was cooled to RT and concentrated in vacuo. The residue was suspended in H2O and filtered. The pad was washed with H2O (2×50 mL) and Et2O (2×50 mL) and the solids were dried in vacuo to furnish the title compound, which was used without further purification. MS (APCI pos) 242 (M+H).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07425631B2uspto-grants-2008_09