Reaktion #2890

ord-b9c8478b753b4132a133ace38f7e208b

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigethe organic layer separated
  2. 2
    ExtraktionThe aqueous layer was extracted with dichloromethane
  3. 3
    WaschenThe combined organic layers were washed
  4. 4
    Sonstigedried
  5. 5
    Sonstigeevaporated
  6. 6
    SonstigeThe residue was purified by flash chromatography

Vorschrift

4-Methyl-5-oxazolecarbonyl chloride (15 g) and N,O-dimethylhydroxylamine hydrochloride (11 g) in dry chloroform (100 ml) were cooled to 0° C. and dry pyridine (28.5 g) was added. The mixture was allowed to warm to room temperature. After 30 minutes aqueous sodium hydrogen carbonate was added and the organic layer separated. The aqueous layer was extracted with dichloromethane. The combined organic layers were washed, dried and evaporated. The residue was purified by flash chromatography to yield the title compound as a white solid. M.p. 59°-60° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05731335uspto-grants-1998_03