反应 #70481

反应方程式

6-piperazin-1-yl-nicotinonitrile

1,4-dichlorophthalazine

Et3N

NMP

→

title compound

收率 51.1%

6-[4-(4-Chloro-phthalazin-1-yl)-piperazin-1-yl]-nicotinonitrile

收率 51.1%

溶剂

H2O

反应条件

后处理

1. 1
   温度Upon cooling to room temperature
2. 2
   其他the precipitate isolated by filtration
3. 3
   洗涤rinsing with additional H2O
4. 4
   其他Crude material is purified by recrystallization (CH2Cl2:heptanes)

实验过程

To a 100-mL round-bottom flask is added 6-piperazin-1-yl-nicotinonitrile (9.60 g, 50 mmol), 1,4-dichlorophthalazine (11.2 g, 55.1 mmol, 1.1 eq), Et3N (3.5 mL, 250 mmol, 5 eq.), and NMP (100 mL). The mixture is heated to 80° C. for 2.5 h. Upon cooling to room temperature, the reaction is poured into H2O (500 mL) and the precipitate isolated by filtration, rinsing with additional H2O. Crude material is purified by recrystallization (CH2Cl2:heptanes) to afford 8.96 g title compound as a beige solid.

来源