反应详情

温度

60 °C

Solid K2CO3 (10 g, 72.4 mmol, 1.8 eq) is added to a solution of (R)-2-methyl-piperazine (4.00 g, 40 mmol, 1 eq) and 3,6-dichloro-4,5-dimethyl-pyridazine (8 g, 45.2 mml, 1.1 eq) in DMF (50 mL), and the resulting solution is stirred at 60° C. for 48 h. The reaction mixture is concentrated to ½ volume under reduced pressure and the minimum water (ca. 15 mL) required to dissolve the solid salts is added, followed by the addition of dichloromethane (100 mL). The organic layer is separated, dried over sodium sulfate and concentrated under reduced pressure, then purified by silica gel column chromatography (2%-20% MeOH/CH2Cl2) to yield the desired compound as a white solid (4.7 g, 49%).

1. concentrationThe reaction mixture is concentrated
2. dissolutionto dissolve the solid salts
3. additionis added
4. additionfollowed by the addition of dichloromethane (100 mL)
5. customThe organic layer is separated
6. dry with materialdried over sodium sulfate
7. concentrationconcentrated under reduced pressure
8. custompurified by silica gel column chromatography (2%-20% MeOH/CH2Cl2)