反应详情

温度

30 °C

The tert-butyl 1′-(6-chloropyrimidin-4-yl)-4,4′-bipiperidine-1-carboxylate (100 mg, 0.26 mmol), phenylmethanol (0.031 mL, 0.29 mmol) were added to DMF (2.6 mL), and then sodium hydride (7 mg, 0.29 mmol) was added to the mixture. The reaction was heated to 30° C. for 30 min The reaction crude was cooled down to r.t. and quenched with ice ammonia chloride solution (10 mL) and extracted with ethyl acetate (10 mL). The organic phase was washed with brine (10 mL, ×1), dried over magnesium sulfate, filtered and concentrated by rotavapor. The crude mixture was purified by preparative TLC with 30% ethylacetate:hexane to yield the title compound.

1. customThe reaction crude
2. temperaturewas cooled down to r.t.
3. customquenched with ice ammonia chloride solution (10 mL)
4. extractionextracted with ethyl acetate (10 mL)
5. washThe organic phase was washed with brine (10 mL, ×1)
6. dry with materialdried over magnesium sulfate
7. filtrationfiltered
8. concentrationconcentrated by rotavapor
9. customThe crude mixture was purified by preparative TLC with 30% ethylacetate