HRID584282

反应详情

EQUATION

反应方程式

HRID 584282 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

7.1 g (53 mmol) of aluminum chloride are placed in 70 ml of nitrobenzene in a round-bottomed flask and under a stream of nitrogen. The mixture is heated at 70° C. until dilution is complete. It is then cooled to 0° C. and 7.2 ml (52 mmol) of 2-propylphenol are added. The mixture is allowed to warm to room temperature and is then heated to 40° C. 4.6 ml (52 mmol) of propionyl chloride are then added dropwise. The reaction medium is heated at 40° C. for 2 hours and then stirred for 48 hours at room temperature. It is then poured into ice with 20 ml of concentrated hydrochloric acid. After extraction with ethyl ether, the organic phase is washed with 2N sodium hydroxide. The aqueous phases are acidified with hydrochloric acid and extracted with ether. The organic phase is dried over magnesium sulfate, filtered and then evaporated. The black solid obtained is triturated in heptane, filtered off and dried. 3.5 g (35%) of the expected product are obtained in the form of a black powder.

WORKUP

后处理

  1. temperatureIt is then cooled to 0° C.
  2. temperatureto warm to room temperature
  3. temperatureis then heated to 40° C
  4. temperatureThe reaction medium is heated at 40° C. for 2 hours
  5. extractionAfter extraction with ethyl ether
  6. washthe organic phase is washed with 2N sodium hydroxide
  7. extractionextracted with ether
  8. dry with materialThe organic phase is dried over magnesium sulfate
  9. filtrationfiltered
  10. customevaporated
  11. customThe black solid obtained
  12. customis triturated in heptane
  13. filtrationfiltered off
  14. customdried