Reaktion #54970

ord-e99868daabbf4ff2a4cdcb3104c95ef8

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationThe reaction mixture was filtered
  2. 2
    Sonstigethe filtrate was evaporated under reduced pressure
  3. 3
    Sonstigeto give a yellow oil
  4. 4
    SonstigeThe oil crystallized from ethanol/hexane

Vorschrift

A solution of 8 g (0.02 mol) N-hydroxy-2-methyl-2-phenyl-4-trichloromethyl-5,5-dichloro-6-oxotetrahydro-1,3-oxazine, 2.4 g (0.02 mol) phenylisocyanate and several drops triethylamine in 90 ml dichloromethane was stirred at about 10° C. for about 2 days. The reaction mixture was filtered and the filtrate was evaporated under reduced pressure to give a yellow oil. The oil crystallized from ethanol/hexane to give 4 g of product, m.p. 154°-157° C. The product is tabulated in Table I as Compound No. 8.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04151279uspto-grants-1979_04