تفاعل #80433

معادلة التفاعل

2-Mercaptobenzimidazole

ethyl 2-dimethylamino-3-(2-chloromethyl-3-methyl-4-pyridylthio)propionate

sodium hydroxide

→

2-((3-methyl-4-(2-dimethylamino-2-ethoxycarbonylethylthio)-2-pyridyl)methylthio)-1H-benzimidazole

المذيبات

ethanol

ظروف التفاعل

المعالجة

1. 1
   تركيزThe reaction mixture was concentrated under reduced pressure and water
2. 2
   workup.ADDITIONwas added to the residue
3. 3
   استخلاصThe mixture was extracted with ethyl acetate
4. 4
   غسيلThe extract was washed with water
5. 5
   تجفيفdried over anhydrous magnesium sulfate
6. 6
   workup.DISTILLATIONthe solvent was distilled away under reduced pressure
7. 7
   غسيلeluted with chloroform-methanol

الإجراء التجريبي

2-Mercaptobenzimidazole (1.5 g) was dissolved in ethanol (20 ml) and thereto were added ethyl 2-dimethylamino-3-(2-chloromethyl-3-methyl-4-pyridylthio)propionate (3.16 g) and an aqueous solution (10 ml) of 1N sodium hydroxide. The mixture was stirred at 50° C. for 1 hour. The reaction mixture was concentrated under reduced pressure and water was added to the residue. The mixture was 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-dimethylamino-2-ethoxycarbonylethylthio)-2-pyridyl)methylthio)-1H-benzimidazole as a pale yellow oil.

المصدر