Reaktion #3843

Reaktionsgleichung

Ethyl acetate

[2-(2-benzoyl-phenyldisulfanyl)-phenyl]phenyl-methanone

Hydroxylamine hydrochloride

HCl

→

title compound

Ausbeute 35.9%

{2-[2-(hydroxyimino-phenyl-methyl)-phenyldisulfanyl]phenyl}-phenyl-methanon

Ausbeute 35.9%

Lösungsmittel

ethanol

pyridine

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe solution was refluxed for 90 minutes
2. 2
   TemperaturThe solution was cooled
3. 3
   Sonstigethe layers were separated
4. 4
   Waschenthe organic portion was washed with brine
5. 5
   Trocknendried (MgSO4)
6. 6
   Filtrationfiltered
7. 7
   EinengenThe filtrate was concentrated to dryness
8. 8
   Sonstigethe residue was triturated with 75% hexane/25% ethyl acetate

Vorschrift

The [2-(2-benzoyl-phenyldisulfanyl)-phenyl]phenyl-methanone (0.55 g, 1.2 mmol) was diluted with ethanol (5 mL) and anhydrous pyridine (5 mL). Hydroxylamine hydrochloride (1 g, 14 mmol) was added and the solution was refluxed for 90 minutes. The solution was cooled and poured into cold aqueous HCl (1N). Ethyl acetate was added, the layers were separated, and the organic portion was washed with brine, dried (MgSO4), and filtered. The filtrate was concentrated to dryness and the residue was triturated with 75% hexane/25% ethyl acetate to give the title compound (0.19 g, 32%) as a white solid, mp 191°-193° C.;

Quelle