Reaktion #1972826

ord-ecc0b4b4a4444506a5322dc30a8772cb

Reaktionsbedingungen

Temperatur
130°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe mixture is heated
  2. 2
    workup.DISTILLATIONAfter 23 hours the excess morpholine is distilled off
  3. 3
    Extraktionthe mixture is extracted with dilute hydrochloric acid
  4. 4
    Extraktionis extracted with toluene
  5. 5
    TrocknenThe toluene solution is dried with K2CO3
  6. 6
    Einengenis concentrated
  7. 7
    SonstigeThe residue, 34.0 g, crystallises out from ethyl acetate with a melting point of 63°-66° C.

Vorschrift

29.43 g (0.15 mol) of 2-(4-fluorophenyl)-3,3-dimethyl-2-methoxyoxirane and 52.3 g (0.60 mol) of morpholine are brought together, and the mixture is heated to reflux temperature (about 130° C.). After 23 hours the excess morpholine is distilled off. The residue is taken up with toluene, and the mixture is extracted with dilute hydrochloric acid. The hydrochloric acid solution is rendered alkaline and is extracted with toluene. The toluene solution is dried with K2CO3 and is concentrated. The residue, 34.0 g, crystallises out from ethyl acetate with a melting point of 63°-66° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05145885uspto-grants-1992_09