Reaktion #3654

Reaktionsgleichung

5,6-dihydro-4H-[1,2,4]triazolo[4,3-a][1,5]benzodiazepine

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

triethylamine

→

desired product

N-[4-(4H-[1,2,4]triazolo[4,3-a][1,5]benzodiazepin-6(5H)-ylcarbonyl)phenyl]-2-methyl benzamide

Lösungsmittel

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Waschenwashed with water, aqueous NaHCO3 and brine
2. 2
   TrocknenThe solution is dried (Na2SO4)
3. 3
   Sonstigethe solvent removed in vacuo
4. 4
   Sonstigeto give a solid
5. 5
   SonstigeThe solid is purified by chromatography on silica gel with ethyl acetate-hexane as solvent

Vorschrift

To a mixture of 5 mmol of 5,6-dihydro-4H-[1,2,4]triazolo[4,3-a][1,5]benzodiazepine in 20 ml of dichloromethane is added 5.5 mmol of 4-[(2-methylbenzoyl)amino]benzoyl chloride and then 7.5 mmol of triethylamine. The mixture is stirred at room temperature for 8 hours and then washed with water, aqueous NaHCO3 and brine. The solution is dried (Na2SO4) and the solvent removed in vacuo to give a solid. The solid is purified by chromatography on silica gel with ethyl acetate-hexane as solvent to give the desired product as a glass.

Quelle