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
81.3 g of acetanilide are suspended in 600 ml of carbon disulphide and 76.7 g of butyryl chloride and, in portions, 198 g of aluminium trichloride are added while stirring. The mixture is stirred for some time at 30°-35° and heated at the boil for 18 hours. It is then allowed to cool, stirred into 200 ml of ice-water and extracted twice with 500 ml of ethyl acetate each time. The organic phases are combined, washed with 500 ml of additional acid and twice with 500 ml of 15% strength sodium carbonate solution each time, dried over magnesium sulphate and concentrated to 150 ml under reduced pressure. The residue obtained by concentration is allowed to cool, filtered with suction, washed twice with diethyl ether and dried under reduced pressure. p-Acetaminobutyrophenone having a melting point of 141°-143° is obtained.
WORKUP
后处理
- stirringThe mixture is stirred for some time at 30°-35°
- temperatureheated at the boil for 18 hours
- temperatureto cool
- extractionextracted twice with 500 ml of ethyl acetate each time
- washwashed with 500 ml of additional acid and twice with 500 ml of 15% strength sodium carbonate solution each time
- dry with materialdried over magnesium sulphate
- concentrationconcentrated to 150 ml under reduced pressure
- customThe residue obtained by concentration
- temperatureto cool
- filtrationfiltered with suction
- washwashed twice with diethyl ether
- customdried under reduced pressure