Reaktion #500697

ord-270be73d92604e87855649e73eeb2f3f

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Einengenafter which the reaction mixture was concentrated in vacuo
  2. 2
    Sonstigeto afford a light brown syrupy, which
  3. 3
    Sonstigecrystallised
  4. 4
    workup.ADDITIONTrituration with a mixture of Et2O/CH2Cl2 3:1
  5. 5
    Filtrationfollowed by filtration
  6. 6
    Waschenwashing

Vorschrift

A stirred solution of 4-(2-aminophenylamino)-2-chloro-2′-methylbenzophenone (3.0 mmol) in glacial acetic acid (5.0 ml) was heated to 70° C., then succinic anhydride (4.0 mmol) was added. The temperature was held at 100° C. for 20 min after which the reaction mixture was concentrated in vacuo to afford a light brown syrupy, which crystallised on standing. Trituration with a mixture of Et2O/CH2Cl2 3:1 followed by filtration and washing yielded the product as white crystals.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06566554B1uspto-grants-2003_05