HRID617226
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
- 50 °C
PROCEDURE
实验过程
A mixture of ethyl 2-iodomethyl-6,7-dimethoxy-4- (3,4-dimethoxyphenyl)quinoline-3-carboxylate (9.0 g), 2-hydroxy-1-methylimidazole (1.8 g), silver carbonate (I) (Ag2CO3) (5.1 g) and benzene (100 ml) was stirred at 50° C. for 18 hours. Then the insoluble materials were filtered off. The filtrate was washed with water, dried (MgSO4), and the solvent was distilled off. The residual oil was subjected to column chromatography on silica gel. From the fraction eluted with chloroform/ethyl acetate (5:1, v/v), ethyl 6,7-dimethoxy-4-(3,4-dimethoxyphenyl)-2-[(1-methyl-2-imidazolyl)oxymethyl]quinoline-3-carboxylate (0.8 g, 9%) was obtained and recrystallized from ethyl acetate/hexane.
WORKUP
后处理
- filtrationThen the insoluble materials were filtered off
- washThe filtrate was washed with water
- dry with materialdried (MgSO4)
- distillationthe solvent was distilled off
- washFrom the fraction eluted with chloroform/ethyl acetate (5:1