Réaction #70481

Équation de réaction

6-piperazin-1-yl-nicotinonitrile

1,4-dichlorophthalazine

Et3N

NMP

→

title compound

Rendement 51.1%

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

Rendement 51.1%

Solvants

H2O

Conditions de réaction

Traitement

1. 1
   TempératureUpon cooling to room temperature
2. 2
   Autrethe precipitate isolated by filtration
3. 3
   Lavagerinsing with additional H2O
4. 4
   AutreCrude material is purified by recrystallization (CH2Cl2:heptanes)

Mode opératoire

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.

Source