反应详情

温度

102.5 °C

A 2 L round-bottom flask was charged with tert-butyl 2,6-diazaspiro[3,3]heptane-6-carboxylate (64.3 g, 0.32 mol), cesium carbonate (317.0 g, 0.97 mol), 2-chloropyrimidine (45.5 g, 0.4 mol), and DMF (759.0 mL). The reaction mixture was heated to 100-105° C. for 20 min. The reaction mixture was cooled to ambient temperature, diluted with water (759.0 mL) and EtOAc (759.0 mL). The organic layer was washed with water (2×500.0 mL) and brine (500.0 mL). The organic layer was dried over sodium sulfate and filtered through Celite™. The filtrate was concentrated under reduced pressure. Column chromatography of the resulting crude product on silica gel, eluting with EtOAc and heptane (50-100%) afforded the desired product.

1. temperatureThe reaction mixture was cooled to ambient temperature
2. washThe organic layer was washed with water (2×500.0 mL) and brine (500.0 mL)
3. dry with materialThe organic layer was dried over sodium sulfate
4. filtrationfiltered through Celite™
5. concentrationThe filtrate was concentrated under reduced pressure
6. washColumn chromatography of the resulting crude product on silica gel, eluting with EtOAc and heptane (50-100%)