Reaktion #70481

Reaktionsgleichung

6-piperazin-1-yl-nicotinonitrile

1,4-dichlorophthalazine

Et3N

NMP

→

title compound

Ausbeute 51.1%

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

Ausbeute 51.1%

Lösungsmittel

H2O

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturUpon cooling to room temperature
2. 2
   Sonstigethe precipitate isolated by filtration
3. 3
   Waschenrinsing with additional H2O
4. 4
   SonstigeCrude material is purified by recrystallization (CH2Cl2:heptanes)

Vorschrift

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.

Quelle