反应详情

1,4-dichlorophthalazine (1 g, 5 mmol) and 2,2-dimethyl piperazine (1.75 g, 15 mmol, 3 eq) were slurried in 5 mL of MEK for 3 h at 45° C. After cooling to rt, the reaction was diluted with 150 mL of dichloromethane and washed with 1×20 mL of sat. NaHCO3 and 1×20 mL of sat. NaCl solution. The organic layer was dried over MgSO4, filtered, and concentrated. Purification by column chromatography (100:5→8:1 dichloromethane:methanol:triethylamine) afforded 1-chloro-4-(3,3-dimethylpiperazin-1-yl)phthalazine. MS (M+H)+=277.0.

1. washwashed with 1×20 mL of sat. NaHCO3 and 1×20 mL of sat. NaCl solution
2. dry with materialThe organic layer was dried over MgSO4
3. filtrationfiltered
4. concentrationconcentrated
5. customPurification by column chromatography (100:5→8:1 dichloromethane:methanol:triethylamine)