HRID1637911
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
PROCEDURE
实验过程
3.1 g (11.2 mmol) of ethyl 4-(bromomethyl)-2-chlorobenzoate are added dropwise to a solution composed of 0.94 g (14.3 mmol) of potassium cyanide, 3.75 ml of water and 8.8 ml of ethanol, heated under reflux. After refluxing for 3 hours, the medium is poured over 200 ml of water, and extracted with ethyl acetate. The organic phase is washed with a dilute HCl solution and then with water saturated with NaCl. The oil obtained after concentration of the organic phase is purified by flash chromatography on silica (hexane-ethyl acetate 1:0 to 1:1 gradient). 0.4 g of a brown solid is obtained (Yield=16%).
WORKUP
后处理
- temperatureheated
- temperatureunder reflux
- temperatureAfter refluxing for 3 hours
- extractionextracted with ethyl acetate
- washThe organic phase is washed with a dilute HCl solution
- customThe oil obtained after concentration of the organic phase
- customis purified by flash chromatography on silica (hexane-ethyl acetate 1:0 to 1:1 gradient)