Reaktion #314736

ord-95d444a5725d4f3d89bff7eb6a69388c

Lösungsmittel

Reaktionsbedingungen

Temperatur
50°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe mixture was heated
  2. 2
    Temperaturat reflux for 1 hour
  3. 3
    Filtrationafter which the precipitated product was filtered off
  4. 4
    Waschenwashed with toluene
  5. 5
    SonstigeDrying in vacuum

Vorschrift

2-Amino-6-chlorobenzoic acid (30 g) was suspended in 1,4-dioxane (225 ml) and ethyl chloroformate (75 ml) was added. The mixture was heated at reflux for 1 hour, then cooled to 50° C., and acetyl chloride (75 ml) was added. The mixture was stirred for 10 hours, after which the precipitated product was filtered off and washed with toluene. Drying in vacuum yields 5-chloroisatoic anhydride (33 g, 97% yield).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07560557B2uspto-grants-2009_07