反応 #3660

反応方程式

10,11-dihydro-10-(3-methyl-4-aminobenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine

2,4-dichlorobenzoyl chloride

diisopropylethylamine

→

crystals

収率 84.1%

N-[4-(5H-Pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)-ylcarbonyl)-2-methylphenyl]-2,4-dichlorobenzamide

収率 84.1%

溶媒

dichloromethane

反応条件

後処理

1. 1
   洗浄The mixture is washed with water
2. 2
   乾燥dried (MgSO4)
3. 3
   濃縮The filtrate is concentrated
4. 4
   workup.ADDITIONhexane added
5. 5
   その他to give crystals
6. 6
   その他Recrystallization from dichloromethane-hexane

実験手順

A mixture of 0.40 g of 10,11-dihydro-10-(3-methyl-4-aminobenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine, 0.40 g of 2,4-dichlorobenzoyl chloride and 0.75 g of diisopropylethylamine in 50 ml of dichloromethane is stirred at room temperature for 16 hours. The mixture is washed with water, dried (MgSO4) and the solution passed through a thin pad of hydrous magnesium silicate. The filtrate is concentrated and hexane added to give crystals. Recrystallization from dichloromethane-hexane gives 0.52 g of crystals, m.p. 213°-215° C.

出典