Reaktion #55351

ord-6572f0c54f304f6b8594fe20750711f6

Lösungsmittel

Reaktionsbedingungen

Temperatur
20°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeat about 25° C
  2. 2
    SonstigeThe product which crystallises
  3. 3
    Filtrationis filtered off
  4. 4
    Waschenwashed with water (6×500 cc.)
  5. 5
    SonstigeAfter drying

Vorschrift

Phenyl chloroformate (126 g.) is added to a suspension of 2-(7-chloro-1,8-naphthyridin-2-yl)-3-hydroxy-isoindolin-1-one (86.5 g.) in pyridine (980 cc.), whilst keeping the temperature at about 25° C. The reaction mixture is stirred for 3 hours at a temperature of about 20° C. and then poured into ice-water (9,000 cc.). The product which crystallises is filtered off, washed with water (6×500 cc.) and then with acetonitrile (3×200 cc.). After drying, 2-(7-chloro-1,8-naphthyridin-2-yl)-3-phenoxycarbonyloxy-isoindolin-1-one (96.7 g.), which melts at 235° C. with decomposition, is obtained.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04220646uspto-grants-1980_09