反应详情

Charge a 250 μL round bottom flask equipped with: a magnetic stirrer, temperature controlled heating mantle, N2 atmosphere, with 7-pyridin-4-yl-imidazo[1,2-a]pyridine (3.35 g, 17.2 mmol), NIS (3.8 g, 16.8 mmol), EtOH (3A). Heat the reaction to 65° C. for 1 hour. This can be followed by SiO2 TLC (100% EtOAc). Add more NIS (3.8 g, 16.8 mmol) and heat the reaction to 65° C. for 1 hour. Mix the reaction while cooling in an ice bath for 30 minutes then filter and rinse the solids with MeOH. Air dry the solids and vacuum oven dry at 40° C. to afford 4.59 g (83%). Additional product can be obtained from the filtrate. MS (ES), m/z 322 (M+1).

1. additionCharge a 250 μL round bottom flask
2. customequipped with: a magnetic stirrer
3. temperatureHeat
4. customthe reaction to 65° C. for 1 hour
5. temperatureheat
6. customthe reaction to 65° C. for 1 hour
7. additionMix
8. customthe reaction
9. temperaturewhile cooling in an ice bath for 30 minutes
10. filtrationthen filter
11. washrinse the solids with MeOH
12. customAir dry the solids and vacuum oven
13. customdry at 40° C.
14. customto afford 4.59 g (83%)
15. customAdditional product can be obtained from the filtrate