HRID1263134

反应详情

EQUATION

反应方程式

HRID 1263134 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

2.8 Grams of 6-(4-chloro-1-butenyl)-3,4- dihydrocarbostyril and 2.1 g of sodium iodide were dissolved in 40 ml of dimethylformamide and stirred at 50° C. for 1 hour. To this solution were added 2.7 g of 4-(2-chloro-6-methlphenyl)piperazine and 1.5 g of triethylamine and the mixture was further stirred at 50° C. for 5 hours. 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 minutes to precipitate crystals. The crystals were separated by a silica-gel chromatography and recrystallized from ethanol-acetone-chloroform to obtain 6-{4-[4-(2-chloro-6-methlphenyl)-1-piperazinyl]-1-butenyl}-3,4-dihydrocarbostyril in colorless prism-like crystals. Yield: 2.7 g. Melting point: 179°-180° C.

WORKUP

后处理

  1. stirringthe mixture was further stirred at 50° C. for 5 hours
  2. concentrationThe reaction mixture was concentrated under a reduced pressure to dryness
  3. customto obtain a residue
  4. stirringstirred at a room temperature for 30 minutes
  5. customto precipitate crystals
  6. customThe crystals were separated by a silica-gel chromatography
  7. customrecrystallized from ethanol-acetone-chloroform