反应详情

Heat a mixture of 3,6-dichloro-4,5-dimethylpyridazine (11.0 g, 62.1 mmol), tert-butyl methyl(piperidin-4-yl)carbamate (23.3 g, 109 mmol), and powdered K2CO3 (17.2 g, 124 mmol) in DMSO (310 mL) at 120° C. for 2 d. Cool the reaction mixture, dilute with H2O, and filter off the solid. Rinse the solid with H2O, and dry under vacuum at 45° C. Dissolve the solid in CH2Cl2, and pass the solution through a pad of silica gel, eluting with CH2Cl2. Concentrate the organic layer under reduced pressure to obtain the title compound as a yellow solid (14.3 g, 65%). ES/MS m/z (35Cl) 355.0 (M+1).

1. temperatureHeat
2. temperatureCool the reaction mixture
3. filtrationfilter off the solid
4. washRinse the solid with H2O
5. customdry under vacuum at 45° C
6. dissolutionDissolve the solid in CH2Cl2
7. washeluting with CH2Cl2
8. concentrationConcentrate the organic layer under reduced pressure