反应详情

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.

1. temperatureis heated on a steam bath for 3 hours
2. washThe mixture is washed with H2O, 1M NaHCO3, H2O, 1N HCl, brine
3. dry with materialdried (Na2SO4)
4. filtrationThe solution is filtered through a thin pad of hydrous magnesium silicate
5. washthe filter cake washed with dichloromethane
6. concentrationThe filtrate is concentrated to dryness under vacuum
7. customthe residue crystallized from dichloromethane-hexane