HRID640683
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
- 70 °C
PROCEDURE
实验过程
To a stirred solution of 2-chloroaniline (1 g. 7.8 mmol.) in acetic acid (10 ml), activated silferc (1.25 g. ferric chloride 7.8 mmol) was added under nitrogen atmosphere. The reaction mixture was stirred for 5 minutes and methyl vinyl ketone (MVK) (0.6 g, 8.5 mmol) was added slowly over a period of 15 minutes. The reaction mixture was heated to 70° C. and maintained between 70-75° C. for one hour. Anhydrous zinc chloride (1.0 g. 7.8 mmol) was added and the reaction was further refluxed for two hours. The reaction mixture was cooled, filtered, basified with 10% NaOH solution, extracted with ethyl acetate (3×20 ml), dried over Na2SO4 and evaporated to give the product; Yield 62%.
WORKUP
后处理
- temperaturemaintained between 70-75° C. for one hour
- temperaturethe reaction was further refluxed for two hours
- temperatureThe reaction mixture was cooled
- filtrationfiltered
- extractionextracted with ethyl acetate (3×20 ml)
- dry with materialdried over Na2SO4
- customevaporated
- customto give the product