反応 #80430

反応方程式

water

ethylene bromohydrin

potassium carbonate

2-((3-Methyl-4-(2-aminoethylthio)-2-pyridyl)methylthio)-1H-benzimidazole

dimethylformamide

→

2-((3-methyl-4-(2-(N,N-bis(2-hydroxyethyl)amino)ethylthio)-2-pyridyl)methylthio)-1H-benzimidazole

反応条件

後処理

1. 1
   抽出extracted with ethyl acetate
2. 2
   洗浄The extract was washed with water
3. 3
   乾燥dried over anhydrous magnesium sulfate
4. 4
   workup.DISTILLATIONthe solvent was distilled away under reduced pressure
5. 5
   洗浄eluted with chloroform-methanol

実験手順

2-((3-Methyl-4-(2-aminoethylthio)-2-pyridyl)methylthio)-1H-benzimidazole (2.0 g) was dissolved in dimethylformamide (20 ml) and thereto were added ethylene bromohydrin (1.59 g) and potassium carbonate (2.1 g). The mixture was stirred at 70°-80° C. for 3 hours. The reaction mixture was poured into water and extracted with ethyl acetate. The extract was washed with water, dried over anhydrous magnesium sulfate and the solvent was distilled away under reduced pressure. The residue was subjected to column chromatography and eluted with chloroform-methanol to give 2-((3-methyl-4-(2-(N,N-bis(2-hydroxyethyl)amino)ethylthio)-2-pyridyl)methylthio)-1H-benzimidazole as a pale yellow oil.

出典