反応 #80427

反応方程式

2-((3-Methyl-4-(2-benzylaminoethylthio)pyridin-2-yl)methylthio)-1H-benzimidazole

methyl chloroacetate

potassium carbonate

→

2-((3-methyl-4-(2-(N-benzyl-N-methoxycarbonylmethylamino)ethylthio)-2-pyridyl)methylthio)-1H-benzimidazole

溶媒

dimethylformamide

反応条件

後処理

1. 1
   その他After the completion of the reaction
2. 2
   workup.DISTILLATIONthe dimethylformamide was distilled away
3. 3
   抽出the residue was extracted with ethyl acetate
4. 4
   乾燥The ethyl acetate layer was dried over anhydrous magnesium sulfate
5. 5
   workup.DISTILLATIONthe solvent was distilled away
6. 6
   その他to give an oily product
7. 7
   その他The oily product was purified by column chromatography

実験手順

2-((3-Methyl-4-(2-benzylaminoethylthio)pyridin-2-yl)methylthio)-1H-benzimidazole (2 g) was dissolved in dimethylformamide and reacted with methyl chloroacetate (0.45 ml) in the presence of potassium carbonate (0.71 g) at 50°-60° C. After the completion of the reaction, the dimethylformamide was distilled away and the residue was extracted with ethyl acetate. The ethyl acetate layer was dried over anhydrous magnesium sulfate and the solvent was distilled away to give an oily product. The oily product was purified by column chromatography to give 2-((3-methyl-4-(2-(N-benzyl-N-methoxycarbonylmethylamino)ethylthio)-2-pyridyl)methylthio)-1H-benzimidazole.

出典