反应详情

温度

0 °C

3-Chloro-4,5-dimethyl-6-[4-(5-trifluoromethyl-pyridin-2-yl)-piperazin-1-yl]-pyridazine (1.0 g, 2.64 mmol), acetonitrile (0.225 mL, 4.22 mmol), and toluene (5 mL) are combined and cooled to 0° C. LiHMDS (8.4 mL, 1.0 M, 8.4 mmol) is added dropwise over 5 min. The reaction is stirred at 0° C. for 1 h, then warmed to room temperature and stirred an additional 16 h. The reaction is quenched by the addition of saturated aq. NH4Cl, and the organics are extracted with EtOAc. The combined organic layers are dried over MgSO4 and concentrated. The residue is purified by flash chromatography on silica gel (0-100% EtOAc in heptanes) to afford the title compound as an orange solid (500 mg, 50%).

1. temperaturewarmed to room temperature
2. stirringstirred an additional 16 h
3. customThe reaction is quenched by the addition of saturated aq. NH4Cl
4. extractionthe organics are extracted with EtOAc
5. dry with materialThe combined organic layers are dried over MgSO4
6. concentrationconcentrated
7. customThe residue is purified by flash chromatography on silica gel (0-100% EtOAc in heptanes)