반응 #3674

반응 방정식

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

triethylamine

2,3-dimethylaniline hydrochloride

diethylphosphoryl cyanide

→

crystals

수율 25.4%

N-(2,3-Dimethylphenyl)-4-(5H-pyrrolo[2,1-c][1,4]-benzodiazepin-10(11H)-ylcarbonyl)benzamide

수율 25.4%

용매

dichloromethane

반응 조건

후처리

1. 1
   온도is heated on a steam bath for 3 hours
2. 2
   세척The mixture is washed with H2O, 1M NaHCO3, H2O, 1N HCl, brine
3. 3
   건조dried (Na2SO4)
4. 4
   여과The solution is filtered through a thin pad of hydrous magnesium silicate
5. 5
   세척the filter cake washed with dichloromethane
6. 6
   농축The filtrate is concentrated to dryness under vacuum
7. 7
   기타the residue 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, 0.222 g of triethylamine, 0.157 g of 2,3-dimethylaniline hydrochloride, 0.15 ml of diethylphosphoryl cyanide in 20 ml of dichloromethane is heated on a steam bath for 3 hours. The mixture is washed with H2O, 1M NaHCO3, H2O, 1N HCl, brine and dried (Na2SO4). The solution is filtered through a thin pad of hydrous magnesium silicate and the filter cake washed with dichloromethane. The filtrate is concentrated to dryness under vacuum and the residue crystallized from dichloromethane-hexane to give 0.11 g of crystals, m.p. 239°-240° C.

출처