HRID428616
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
- 92.5 °C
PROCEDURE
实验过程
A mixture of 2,3-dimethylanisole (2.0 g), 3-(3-benzyl-3H-imidazol-4-yl)-acrylic acid (3.4 g) and methanesulfonic acid (60 ml) is heated at 90-95° C. for 45 minutes. The cooled reaction mixture is poured into water and is made alkaline with sodium hydroxide solution. The product is extracted into ethyl acetate which is washed with water, dried with sodium sulfate and evaporated in reduced pressure. The crude product is purified by flash chromatography by eluting with methylene chloride-methanol solution. The yield is 1.1 g.
WORKUP
后处理
- customThe cooled reaction mixture
- extractionThe product is extracted into ethyl acetate which
- washis washed with water
- dry with materialdried with sodium sulfate
- customevaporated in reduced pressure
- customThe crude product is purified by flash chromatography
- washby eluting with methylene chloride-methanol solution