HRID905139

反应详情

EQUATION

反应方程式

HRID 905139 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

21 g (0.15 mol) of potassium carbonate were added in portions to a suspension of 14.5 g (0.05 mol) of 1-n-propyl-piperazine dihydrobromide in 200 ml of acetonitrile. 7.4 g (0.05 mol) of dichloroacetyl chloride were added dropwise to this mixture at room temperature, while stirring. The mixture was subsequently stirred at 20° C. for 5 hours and working up was then effected by a procedure in which the reaction mixture was filtered and the filtrate was evaporated under reduced pressure. The residue was recrystallized from a mixture of toluene and petroleum ether. 11.5 g (96% of theory) of 1-dichloroacetyl-4-n-propyl-piperazine were obtained in the form of beige-colored crystals of melting point 88° C.

WORKUP

后处理

  1. stirringThe mixture was subsequently stirred at 20° C. for 5 hours
  2. filtrationwas filtered
  3. customthe filtrate was evaporated under reduced pressure
  4. customThe residue was recrystallized from a mixture of toluene and petroleum ether