反应详情

温度

0 °C

4-Pyridylacetonitrile hydrochloride (5.00 g, 32.3 mmol) in 40 mL of THF was sonicated for 10 min, and the mixture was added to 10 mL THF solution of NaH (1.55 g, 64.7 mmol) using dripping funnel while the temperature was kept below 15° C. After the addition, the mixture was cooled to 0° C. and 1,4-dichlorophthalazine (3.22 g, 24.3 mmol) was added to the mixture. The mixture turned into red instantly. The reaction was continued for another 4 hrs, and the mixture was poured in cold NH4Cl solution. The resulting red solid was filtered, washed with H2O, and dried to give 4.4 g of 1-chloro-4-(4-pyridylcyanomethyl)phthalazine (65%); mp 265° C. (dec); 1H NMR (CDCl3) δ 6.00 (s, 1H), 7.39-8.60 (m, 8H); LC/MS MH+281.4.

1. customwas kept below 15° C
2. additionAfter the addition
3. filtrationThe resulting red solid was filtered
4. washwashed with H2O
5. customdried