反応 #3655

反応方程式

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

溶媒

dichloromethane

dichloromethane

反応条件

後処理

1. 1
   洗浄washed with water, aqueous NaHCO3 and brine
2. 2
   乾燥The organic layer is dried (Na2SO4)
3. 3
   その他the solvent removed under vacuum
4. 4
   その他The residue is purified by chromatography on silica gel

実験手順

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.

出典