HRID2291191

反应详情

EQUATION

反应方程式

HRID 2291191 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

1.9 Grams of 6-{1-hydroxy-4-[4-(3-chlorophenyl)-1-piperazinyl]butyl}-3,4-dihydrocarbostyril was dissolved in 50 ml of acetic acid and further 2 ml of concentrated hydrochloric acid was added to this solution. The solution was stirred at 80° C. for 30 minutes and the reaction mixture was concentrated under a reduced pressure to dryness to obtain a residue. To the residue were added 10N-NaOH and ether and stirred at a room temperature for 30 minues. The crystals thus precipitated were collected by filtration and separated by a silica-gel chromatography. Recrystallized from ethanol-chloroform to obtain 6-{4-[4-(3-chlorophenyl)-1-piperazinyl]-1-butenyl}-3,4-dihydrocarbostyril in colorless prism-like crystals. Yield: 1.6 g. Melting point: 175°-176° C.

WORKUP

后处理

  1. concentrationthe reaction mixture was concentrated under a reduced pressure to dryness
  2. customto obtain a residue
  3. stirringstirred at a room temperature for 30 minues
  4. customThe crystals thus precipitated
  5. filtrationwere collected by filtration
  6. customseparated by a silica-gel chromatography
  7. customRecrystallized from ethanol-chloroform