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
A mixture of 158 g of 3-chlorobenzaldehyde, 111.6 g of trimethylsilylnitrile and a catalytic amount of zinc iodide was heated at 90° C. for 2 hours, with stirring. The reaction mixture was ice-cooled, and 350 ml of concentrated aqueous hydrochloric acid were added to it. The resulting mixture was then heated under reflux for 1 hour, after which it was mixed with water and with ethyl acetate. The ethyl acetate layer was separated and mixed with a 30% w/v aqueous solution of sodium hydroxide. The aqueous layer was separated, washed three times with ethyl acetate and then acidified with concentrated aqueous hydrochloric acid, after which it was extracted with ethyl acetate. The extract was washed with water and dried over anhydrous sodium sulfate. The solvent was then removed by distillation under reduced pressure, to give the title compound as crystals, melting at 110°-114° C.
WORKUP
后处理
- temperaturecooled
- temperatureThe resulting mixture was then heated
- temperatureunder reflux for 1 hour
- customThe ethyl acetate layer was separated
- additionmixed with a 30% w/v aqueous solution of sodium hydroxide
- customThe aqueous layer was separated
- washwashed three times with ethyl acetate
- extractionafter which it was extracted with ethyl acetate
- washThe extract was washed with water
- dry with materialdried over anhydrous sodium sulfate
- customThe solvent was then removed by distillation under reduced pressure