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 ethyl acetate and 2N hydrochloric acid (to give pH 3-4), and the layers separated. The organic phase was washed with brine, concentrated under reduced pressure, redissolved in ethyl acetate, dried (MgSO4) 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 ethyl acetate and 2N hydrochloric acid (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 ethyl acetate
9. dry with materialdried (MgSO4)
10. customevaporated under reduced pressure