Reaktion #449580

ord-1c7abc3565f04744bcbd217f30409c58

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Waschenwashed with H2O 1N HCl, 1M NaHCO3, brine
  2. 2
    Trocknendried (Na2SO4)
  3. 3
    SonstigeThe solvent is removed
  4. 4
    Sonstigeto give a solid
  5. 5
    Filtrationfiltered through a thin pad of hydrous magnesium silicate with dichloromethane as eluent

Vorschrift

To a mixture of 0.362 g of 4-[(6,11-dihydro-5H-dibenz[b,e]azepin-5-yl)carbonyl]benzoyl chloride and 0.101 g of triethylamine in 5 ml of dichloromethane is added a solution of 0.129 g of 2-methylaniline in 3 ml of dichloromethane. The mixture is stirred 1.5 hr at room temperature and then washed with H2O 1N HCl, 1M NaHCO3, brine and dried (Na2SO4). The solvent is removed to give a solid. The solid is dissolved in dichloromethane and filtered through a thin pad of hydrous magnesium silicate with dichloromethane as eluent to give 0.025 g of crystals, m.p. 214°-216° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05869483uspto-grants-1999_02