Реакция #3843

ord-169cfd162f7a4903b732bbd90fedb229

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураthe solution was refluxed for 90 minutes
  2. 2
    ТемператураThe solution was cooled
  3. 3
    Другоеthe layers were separated
  4. 4
    Промывкаthe organic portion was washed with brine
  5. 5
    Сушкаdried (MgSO4)
  6. 6
    Фильтрацияfiltered
  7. 7
    КонцентрированиеThe filtrate was concentrated to dryness
  8. 8
    Другоеthe residue was triturated with 75% hexane/25% ethyl acetate

Методика

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.;

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05734081uspto-grants-1998_03