HRID1182374

反应详情

EQUATION

反应方程式

HRID 1182374 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
112 °C

PROCEDURE

实验过程

500 mg (2.1865 mmol) 6-chloro-4-o-tolyl-nicotinonitrile were dissolved in 10.0 ml toluene and heated to 112° C. At this temperature 2.19 g (21.865 mmol) 1-methylpiperazine were added, and the reaction mixture was stirred for further 60 minutes. The mixture was cooled down to 50° C. and concentrated under reduced pressure. 5 ml toluene were added to the obtained residue at a temperature of 20-25° C., followed by 900 mg sulfuric acid (95%). The organic phase was washed with 5 ml water. Evaporation in vacuo gave 520 mg of 6-(4-methyl-piperazin-1-yl)-4-o-tolyl-nicotinonitrile as a beige foam.

WORKUP

后处理

  1. temperatureThe mixture was cooled down to 50° C.
  2. concentrationconcentrated under reduced pressure
  3. addition5 ml toluene were added to the obtained residue at a temperature of 20-25° C.
  4. washThe organic phase was washed with 5 ml water
  5. customEvaporation in vacuo