反应详情

温度

100 °C

tert-Butyl carbamate (215 mg), cesium carbonate (1.14 g), Pd2(dba)3 (240 mg), and Xantphos (303 mg) were added to a toluene solution (9 ml) containing 2-chloro-3-fluoro-4-iodopyridine (450 mg), followed by stirring at 100° C. for 3 hours. The reaction solution was adjusted to room temperature and water was added to the reaction solution, followed by extraction with ethyl acetate. The organic layers were washed with saturated saline, dried over anhydrous sodium sulfate. Next, the solvent was distilled away under reduced pressure and the obtained residue was purified by silica gel chromatography (n-hexane:ethyl acetate=9:1 to 3:1). A yellow oily matter of tert-butyl (2-chloro-3-fluoropyridin-4-yl)carbamate (533 mg) was thus obtained.

1. customwas adjusted to room temperature
2. extractionfollowed by extraction with ethyl acetate
3. washThe organic layers were washed with saturated saline
4. dry with materialdried over anhydrous sodium sulfate
5. distillationNext, the solvent was distilled away under reduced pressure
6. customthe obtained residue was purified by silica gel chromatography (n-hexane:ethyl acetate=9:1 to 3:1)