HRID1632509

反应详情

EQUATION

反应方程式

HRID 1632509 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. stirringThe mixture is stirred for some time at 30°-35°
  2. temperatureheated at the boil for 18 hours
  3. temperatureto cool
  4. extractionextracted twice with 500 ml of ethyl acetate each time
  5. washwashed with 500 ml of additional acid and twice with 500 ml of 15% strength sodium carbonate solution each time
  6. dry with materialdried over magnesium sulphate
  7. concentrationconcentrated to 150 ml under reduced pressure
  8. customThe residue obtained by concentration
  9. temperatureto cool
  10. filtrationfiltered with suction
  11. washwashed twice with diethyl ether
  12. customdried under reduced pressure