Reaktion #63600

ord-377a94b0686f4107959ba1575d2f4d81

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.STIRRINGAfter stirring for 30 minutes
  2. 2
    workup.STIRRINGUpon completion, stirring
  3. 3
    FiltrationThe precipitated product was filtered off
  4. 4
    Waschenwashed with a lot of water
  5. 5
    Sonstigedried

Vorschrift

To a stirred and cooled (about 10° C.) solution of 11.7 parts of 2-methoxy-5-(trifluoromethyl)benzenamine in 50 parts of acetic acid were added dropwise 7.7 parts of chloroacetyl chloride at a temperature below 20° C. After stirring for 30 minutes, there was added dropwise a solution of 24.8 parts of sodium acetate in 62 parts of water (exothermic reaction). Upon completion, stirring was continued for 30 minutes at room temperature. The precipitated product was filtered off, washed with a lot of water and dried, yielding 15.5 parts (93.3%) of 2-chloro-N-[2-methoxy-5-(trifluoromethyl)phenyl]-acetamide; mp. 94.7° C. (intermediate 62).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04766125uspto-grants-1988_08