反応 #3657

反応方程式

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

4-[(2,4-dichlorobenzoyl)amino]benzoyl chloride

triethylamine

→

desired product

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

溶媒

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 in vacuo
4. 4
   その他to give a solid
5. 5
   その他The solid is purified by chromatography on silica gel

実験手順

To a mixture of 5 mmol of 5,6-dihydro-1-methyl-4H-[1,2,4]triazolo[4,3-a][1,5]benzodiazepine in 20 ml of dichloromethane is added 5.5 mmol of 4-[(2,4-dichlorobenzoyl)amino]benzoyl chloride and 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 organic layer is dried (Na2SO4) and the solvent removed in vacuo to give a solid. The solid is purified by chromatography on silica gel to give the desired product as a solid.

出典