HRID2291032

反应详情

EQUATION

反应方程式

HRID 2291032 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.66 g (0.0152 mole) of sodium hydride (55% strength in liquid paraffin) is added to 2.1 g (0.0131 mole) of 4-(pyrazol-1-yl)-phenol in 60 ml of absolute dimethylformamide, and the mixture is stirred for 1 hour at room temperature. 3.99 g (0.0131 mole) of 1-(3-chloropropyl)-4-(4-fluorophenyl)-piperazine are added, the reaction mixture is stirred for 3 hours at 90° C., under nitrogen as a protective gas, cooled and poured onto ice water, and the precipitate is filtered off under suction. The crude product is recrystallized from ethanol and a product of melting point 151°-153° C. is obtained (yield: 72%).

WORKUP

后处理

  1. stirringthe reaction mixture is stirred for 3 hours at 90° C., under nitrogen as a protective gas
  2. temperaturecooled
  3. additionpoured onto ice water
  4. filtrationthe precipitate is filtered off under suction
  5. customThe crude product is recrystallized from ethanol
  6. customa product of melting point 151°-153° C. is obtained (yield: 72%)