Reaktion #520583

ord-881d7952ef3f41b5ae11a0f0a5d6856d

Lösungsmittel

Reaktionsbedingungen

Temperatur
60°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturAfter cooling to 23° C.
  2. 2
    Waschenwashed with several portions of brine
  3. 3
    Trocknendried over Na2SO4

Vorschrift

A solution of 5-(N-Boc-amino)-5,7-dihydro-6H-dibenz[b,d]azepin-6-one (0.2 g, 0.617 mmol) (Example 7-E) in DMF was treated with Cs2CO3 (0.3 g, 0.925 mmol) and warmed to 60° C. To the reaction mixture was added 1-chloro-3,3-dimethyl-2-butanone (0.096 ml, 0.74 mmol) (Aldrich) and stirring continued for 17 h. After cooling to 23° C., the mixture was diluted with CH25Cl2, washed with several portions of brine and dried over Na2SO4. The title compound was isolated as a colorless solid. C25H30N2O4 (MW=422.522); mass spectroscopy (MH+) 423

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06667305B1uspto-grants-2003_12