反应详情

温度

100 °C

5-Azido-2-fluoropyridine (262 mg, 1.9 mmol) and vinyl acetate (4.0 mL, 43 mmol) were mixed in a flame dried high pressure sealable vessel. The reaction vessel was evacuated and charged with nitrogen, sealed, and heated to 100° C. for 15 hours. The reaction was cooled to room temperature and TLC indicated that the reaction was complete. Minimal dichloromethane was added to the reaction (just enough to dissolve solids that formed upon cooling) and the solution directly chromatographed on silica gel (Biotage size 40S column), eluting with 20-50% ethyl acetate/heptane to give the title compound as a white solid.

1. customdried high pressure sealable vessel
2. customThe reaction vessel was evacuated
3. additioncharged with nitrogen
4. customsealed
5. temperatureThe reaction was cooled to room temperature
6. additionMinimal dichloromethane was added to the reaction (just enough
7. dissolutionto dissolve solids that
8. customformed
9. temperatureupon cooling) and the solution
10. customdirectly chromatographed on silica gel (Biotage size 40S column)
11. washeluting with 20-50% ethyl acetate/heptane