Reaktion #84566

ord-b3862ce897db4dd98957ca235176814c

Lösungsmittel

Reaktionsbedingungen

Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe mixture was cooled to rt
  2. 2
    Einengenconcentrated in vacuo
  3. 3
    SonstigeThe residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=1:4)

Vorschrift

A mixture of 4-(4-amino-2-fluorophenyl)morpholin-3-one (2.51 g, 11.9 mmol) and acetyl ketene (2.51 g, 29.9 mmol) in EtOAc (40 mL) was stirred at 80° C. for 24 h. The mixture was cooled to rt and concentrated in vacuo. The residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=1:4) to give the title compound as a yellow solid (2.15 g, 61%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09434695B2uspto-grants-2016_09