Reaktion #3655

Reaktionsgleichung

4-nitrobenzoyl chloride

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

triethylamine

→

desired product

5,6-Dihydro-6-(4-nitrobenzoyl)-4H-[1,2,4]triazolo[4,3-a][1,5]benzodiazepine

Lösungsmittel

dichloromethane

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Waschenwashed with water, aqueous NaHCO3 and brine
2. 2
   TrocknenThe organic layer is dried (Na2SO4)
3. 3
   Sonstigethe solvent removed under vacuum
4. 4
   SonstigeThe residue is purified by chromatography on silica gel

Vorschrift

To a mixture of 3 mmol of 5,6-dihydro-4H-[1,2,4]-triazolo[4,3-a][1,5]benzodiazepine in 10 ml of dichloromethane under argon is added 5 mmol of triethylamine. To the mixture is added dropwise 3.3 mmol of 4-nitrobenzoyl chloride in 3 ml of dichloromethane. The mixture is stirred at room temperature 3 hours and then washed with water, aqueous NaHCO3 and brine. The organic layer is dried (Na2SO4) and the solvent removed under vacuum. The residue is purified by chromatography on silica gel to give the desired product as a solid.

Quelle