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, 0.111 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.

1. temperatureis heated on a steam bath overnight
2. washThe mixture is washed with water, 1M NaHCO3, 1N HCl, brine
3. dry with materialdried (Na2SO4)
4. filtrationThe dichloromethane solution is filtered through a thin pad of hydrous magnesium silicate
5. concentrationthe filtrate concentrated to dryness
6. customThe residue is crystallized from dichloromethane-hexane