HRID1248575

反应详情

EQUATION

反应方程式

HRID 1248575 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A mixture of 37.8 g (0.15 mole) of 1-(diphenylmethyl)-piperazine, 27.5 g (0.2 mole) of 2-(2-chloroethoxy)-acetamide and 26.5 g of anhydrous sodium carbonate in 120 ml of xylene is heated for 4 hours to 90° to 120° C. Thereafter, 120 ml of benzene are added to the reaction mixture, the precipitate formed is filtered off and the organic phase is extracted with dilute hydrochloric acid (30 ml of concentrated hydrochloric acid and 100 ml of water). 40 ml of a concentrated aqueous solution of sodium hydroxide are added, followed by extraction with benzene. The benzene solution is washed with water, dried over anhydrous sodium carbonate and the benzene is evaporated off to dryness. The evaporation residue is triturated with diethyl ether and left to crystallize. 2-[2-[4-(Diphenylmethyl)-1-piperazinyl]ethoxy]-acetamide is obtained in a yield of 73% of theory; M.P. 119°-120° C.

WORKUP

后处理

  1. customthe precipitate formed
  2. filtrationis filtered off
  3. extractionthe organic phase is extracted with dilute hydrochloric acid (30 ml of concentrated hydrochloric acid and 100 ml of water)
  4. addition40 ml of a concentrated aqueous solution of sodium hydroxide are added
  5. extractionfollowed by extraction with benzene
  6. washThe benzene solution is washed with water
  7. dry with materialdried over anhydrous sodium carbonate
  8. customthe benzene is evaporated off to dryness
  9. customThe evaporation residue is triturated with diethyl ether
  10. waitleft
  11. customto crystallize