反应详情

2-Chloronicotinic acid (10.0 g, 63.5 mmol) was added to a solution of sodium (3 g, 130 mmol) in butanol (100 ml) at 80° C., and the resulting mixture heated under reflux for 4 hours. The reaction was allowed to cool, and partitioned between EtOAc and 2M HCl (to give pH 3-4), and the layers separated. The organic phase was washed with brine, concentrated under reduced pressure, redissolved in EtOAc, dried (MgSO4), filtered and evaporated under reduced pressure, to give the desired product as a solid (11.9 g).

1. temperaturethe resulting mixture heated
2. temperatureunder reflux for 4 hours
3. temperatureto cool
4. custompartitioned between EtOAc and 2M HCl (to give pH 3-4)
5. customthe layers separated
6. washThe organic phase was washed with brine
7. concentrationconcentrated under reduced pressure
8. dissolutionredissolved in EtOAc
9. dry with materialdried (MgSO4)
10. filtrationfiltered
11. customevaporated under reduced pressure