反应详情

温度

80 °C

NaN3 was added to a solution under N2 of 4-chloro-1-(3,5-dichloro-pyridin4-ylmethyl)-6-methoxy-phthalazine (1 g, 2.82 mmoles), obtained as described in example 13, in anhydrous DMF (20 ml) and the mixture was heated at 80° C. overnight, then at 120° C. for 7 hours, then poured into water (10 volumes) and extracted 3 times with CH2Cl2, dried and concentrated under vacuum to give a solid which was purified by flash chromatography (eluent:60:80 petrolatum/ethyl acetate 6:4). The eluate was crystallised from acetonitrile (75 ml) to give 0.36 g of the title compound (yield: 78.5%). m. p.: 275-276° C.

1. customobtained
2. extractionextracted 3 times with CH2Cl2
3. customdried
4. concentrationconcentrated under vacuum
5. customto give a solid which
6. customwas purified by flash chromatography (eluent:60:80 petrolatum/ethyl acetate 6:4)
7. customThe eluate was crystallised from acetonitrile (75 ml)