반응 #3673

반응 방정식

4-(5H-pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)-ylcarbonyl)benzoic acid

triethylamine

o-toluidine

diethylphosphoryl cyanide

→

white crystals

수율 54.6%

N-(2-Methylphenyl)-4-(5H-pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)-ylcarbonyl)benzamide

수율 54.6%

용매

dichloromethane

반응 조건

후처리

1. 1
   온도is heated on a steam bath overnight
2. 2
   세척The mixture is washed with water, 1M NaHCO3, 1N HCl, brine
3. 3
   건조dried (Na2SO4)
4. 4
   여과The dichloromethane solution is filtered through a thin pad of hydrous magnesium silicate
5. 5
   농축the filtrate concentrated to dryness
6. 6
   기타The residue is crystallized from dichloromethane-hexane

실험 절차

A mixture of 0.332 g of 4-(5H-pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)-ylcarbonyl)benzoic acid, 0.111 g of triethylamine, 0.107 g of o-toluidine, and 0.15 ml of diethylphosphoryl cyanide in 20 ml of dichloromethane is heated on a steam bath overnight. The mixture is washed with water, 1M NaHCO3, 1N HCl, brine and dried (Na2SO4). The dichloromethane solution is filtered through a thin pad of hydrous magnesium silicate and the filtrate concentrated to dryness. The residue is crystallized from dichloromethane-hexane to give 0.23 g of white crystals, m.p. 228°-231° C.

출처