反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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 was added 10N-NaOH and ether and stirred at a room temperature for 30 minutes. 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
- concentrationthe reaction mixture was concentrated under a reduced pressure to dryness
- customto obtain a residue
- stirringstirred at a room temperature for 30 minutes
- customThe crystals thus precipitated
- filtrationwere collected by filtration
- customseparated by a silica-gel chromatography
- customRecrystallized from ethanol-chloroform