反应详情

Heat a mixture of potassium carbonate (21.23 g, 153 6 mmol), 1,4-dichlorophthalazine (26 g, 128 mmol) and methyl-piperidin-4-yl carbamic acid tert-butyl ester (30.01 g, 134.4 mmol) in N-methylpyrrolidine (200 mL) at 80° C. overnight. Pour the reaction mixture into water, extract with dichloromethane, dry over Na2SO4, and concentrate under reduced pressure. Add diethylether and filter off the resulting solid (4-chlorophethalazin-1-ol from starting material impurity). Concentrate the filtrate. Purify the resulting residue by flash silica gel chromatography (hexane:ethyl acetate=2:1) to provide the title compound as a white solid (17.66 g, 37%). ES/MS m/z (37Cl) 377.0 (M+1).

1. temperatureHeat
2. extractionextract with dichloromethane
3. dry with materialdry over Na2SO4
4. concentrationconcentrate under reduced pressure
5. filtrationAdd diethylether and filter off the resulting solid (4-chlorophethalazin-1-ol from starting material impurity)
6. concentrationConcentrate the filtrate
7. customPurify the resulting residue by flash silica gel chromatography (hexane:ethyl acetate=2:1)