反应详情

温度

80 °C

To a solution of 3-(4-fluorophenoxy)azetidine (557 mg, 3.37 mmol) [prepared as described in Example AAA] in isopropanol (10 mL, 3 mL/mmol) was added DIPEA (1.5 mL, 8.42 mmol) and 2,4-dichloropyridine (500 mg, 3.37 mmol) and the mixture was heated at 80° C. for 7 h. The reaction mixture was concentrated under reduced pressure and extracted with EtOAc (2×20 mL). The organic extracts were washed with brine, dried over sodium sulfate and concentrated under reduced pressure. Purification by silica gel column chromatography provided 2-chloro-6-(3-(4-fluorophenoxy)azetidin-1-yl)pyridine (500 mg, 55%) as a solid. Observed mass (M+1): 279.1.

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. extractionextracted with EtOAc (2×20 mL)
3. washThe organic extracts were washed with brine
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated under reduced pressure
6. customPurification by silica gel column chromatography