تفاعل #70481

معادلة التفاعل

6-piperazin-1-yl-nicotinonitrile

1,4-dichlorophthalazine

Et3N

NMP

→

title compound

المردود 51.1%

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

المردود 51.1%

المذيبات

H2O

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةUpon cooling to room temperature
2. 2
   أخرىthe precipitate isolated by filtration
3. 3
   غسيلrinsing with additional H2O
4. 4
   أخرىCrude material is purified by recrystallization (CH2Cl2:heptanes)

الإجراء التجريبي

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.

المصدر