反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
In 300 ml of dimethylformamide were dissolved 89 g of 6-(3-chloropropoxy)-3,4-dihydrocarbostyril and 110 g of 1-(4-bromo-2-methylphenyl)-2-mercaptoimidazole. To the solution was slowly added 66.7 g of potassium carbonate at room temperature. The mixture was stirred at 80° C. for 2 hours to give rise to a reaction. After the completion of the reaction, the reaction mixture was extracted with ethyl acetate. The oily layer was washed with water thoroughly, washed with an aqueous solution saturated with sodium chloride, dried with anhydrous magnesium sulfate, and subjected to distillation to remove the solvent. The resulting brown oil was purified by a silica gel column chromatography (eluant: chloroform/methanol=50/1). The resulting crude crystals were recrystallized from ethanol to obtain 118 g of 6-{3-[1-(2-methyl-4-bromophenyl)-2-imidazolylthio]propoxy}-3,4-dihydrocarbostyril.
WORKUP
后处理
- customat room temperature
- customto give rise
- customto a reaction
- customAfter the completion of the reaction
- extractionthe reaction mixture was extracted with ethyl acetate
- washThe oily layer was washed with water thoroughly
- washwashed with an aqueous solution saturated with sodium chloride
- dry with materialdried with anhydrous magnesium sulfate
- distillationsubjected to distillation
- customto remove the solvent
- customThe resulting brown oil was purified by a silica gel column chromatography (eluant: chloroform/methanol=50/1)
- customThe resulting crude crystals were recrystallized from ethanol