反应详情

温度

120 °C

1,4-Dioxa-8-azaspiro[4.5]decane (2.39 g) is combined with 2,5-dichloropyrimidine (2.44 g) in N,N-dimethylformamide (50 mL), 1,4-dioxane (75 mL) and triethylamine (6.7 mL) in a glass pressure reaction vessel. The mixture is heated with stirring at 120° C. for 16 h. After cooling to room temperature, the solution is concentrated and partitioned between dichloromethane (100 mL) and water (100 mL). The aqueous layer is extracted with dichloromethane (100 mL). The dichloromethane layers are combined, washed with water (2×100 mL), dried over Na2SO4, filtered and concentrated to yield the title compound.

1. temperatureThe mixture is heated
2. temperatureAfter cooling to room temperature
3. concentrationthe solution is concentrated
4. custompartitioned between dichloromethane (100 mL) and water (100 mL)
5. extractionThe aqueous layer is extracted with dichloromethane (100 mL)
6. washwashed with water (2×100 mL)
7. dry with materialdried over Na2SO4
8. filtrationfiltered
9. concentrationconcentrated