HRID1263115

反应详情

EQUATION

反应方程式

HRID 1263115 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

5.0 Grams of 6-(1-oxo-4-chlorobutyl)-3,4-dihydrocarbostyril and 7.5 g of sodium iodide were dispersed in 120 ml of anhydrous dimethylformamide and the mixture was stirred at 50°-60° C. for 2 hours. To this reaction mixture were added 10 g of 4-(3-chlorophenyl)piperazine and 5 ml of triethylamine and was stirred at 50°-60° C. for 6 hours, then stirred at a room temperature for 24 hours. The reaction mixture was concentrated under a reduced pressure to obtain a residue. To the residue thus obtained was added 80 ml of 5%-sodium hydrogencarbonate solution and the organic layer was extracted with chloroform. The chloroform layer was washed with water, dried and chloroform was removed by distillation. The residue thus obtained was crystallized with ether to obtain crude crystals and the crude crystals were recrystallized from ethanol to obtain 6.5 g of 6-{1-oxo-4-[4-(3-chlorophenyl)-1-piperazinyl]butyl}-3,4-dihydrocarbostyril in colorless needle-like crystals.

WORKUP

后处理

  1. stirringwas stirred at 50°-60° C. for 6 hours
  2. stirringstirred at a room temperature for 24 hours
  3. concentrationThe reaction mixture was concentrated under a reduced pressure
  4. customto obtain a residue
  5. customTo the residue thus obtained
  6. extractionthe organic layer was extracted with chloroform
  7. washThe chloroform layer was washed with water
  8. customdried
  9. customchloroform was removed by distillation
  10. customThe residue thus obtained
  11. customwas crystallized with ether
  12. customto obtain crude crystals
  13. customthe crude crystals were recrystallized from ethanol