Reaktion #449558

Reaktionsgleichung

4-[(2-methylbenzoyl)amino]benzoyl chloride

6,11-dihydro-5H-dibenz[b,e]azepine

triethylamine

→

white solid

Ausbeute 108.7%

N-[4-[(6,11-Dihydro-5H-dibenz[b,e]azepin-5-yl)carbonyl]phenyl]-2-methylbenzamide

Ausbeute 108.7%

Lösungsmittel

tetrahydrofuran

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigethe solvent removed under vacuum
2. 2
   workup.ADDITIONTo the residue is added 1N HCl
3. 3
   Extraktionthe mixture extracted with ethyl acetate (20 ml)
4. 4
   Waschenthe extract washed with saturated NaHCO3, brine
5. 5
   Trocknendried (Na2SO4)
6. 6
   FiltrationThe solution is filtered through a thin pad of hydrous magnesium silicate
7. 7
   Sonstigethe filtrate evaporated
8. 8
   SonstigeThe residue is triturated with ether-hexane
9. 9
   Filtrationfiltered

Vorschrift

To a solution of 0.27 g (1 mmol) of 4-[(2-methylbenzoyl)amino]benzoyl chloride in 2 ml of tetrahydrofuran is added 0.20 g (1 mmol) of 6,11-dihydro-5H-dibenz[b,e]azepine and 0.20 g of triethylamine. The mixture is stirred at room temperature for 3 hours and the solvent removed under vacuum. To the residue is added 1N HCl and the mixture extracted with ethyl acetate (20 ml) and the extract washed with saturated NaHCO3, brine and dried (Na2SO4). The solution is filtered through a thin pad of hydrous magnesium silicate and the filtrate evaporated. The residue is triturated with ether-hexane and filtered to give 0.47 g of a white solid: Mass Spectrum; EI 433 (M+1); EI-high resolution 432.1842.

Quelle