反应详情

温度

120 °C

A solution of 0.2 g (1.82 mmol) resorcinol in 5 ml dioxane is spiked with 0.37 ml 5.4 M methanolic sodium methylate solution (2 mmol) The crystalline residue is then suspended in 5 ml dioxane, 0.511 g (2 mmol) 1-chloro-4-(4-pyridylmethyl)phthalazine is added, and the reaction mixture stirred under nitrogen atmosphere for 18 h at 120° C. After cooling to RT and filtration, the filtrate is evaporated under vacuum, and the residue purified by means of flash chromatography on silica gel with particle size 0.04-0.06 mm, using acetate and ethyl acetate/methanol mixtures (50:1 and 25:1). The product-containing fractions are evaporated under vacuum, the crystalline residue suspended in about 5 ml dichloromethane, and filtered. Title compound is obtained after drying of the crystallizate under HV (6 h, 100° C.); m.p. 206-207° C.; ESI-MS: (M+H)+=330.

1. temperatureAfter cooling to RT
2. filtrationfiltration
3. customthe filtrate is evaporated under vacuum
4. customthe residue purified by means of flash chromatography on silica gel with particle size 0.04-0.06 mm
5. customThe product-containing fractions are evaporated under vacuum
6. filtrationfiltered