反应详情

温度

60 °C

6-Nitro-4-chloro-2-(3-fluorophenyl)-quinoline 3.2 g (9.50 mmoles) was placed in a 250 mL three neck round bottom flask equipped with a condenser, magnetic stirrer, silicone oil heating bath, nitrogen inlet and gas outlet. To this was added 75 mL of N-methyl pyrrolidinone then 6.0 g (95 mmoles, 10 equiv.) of sodium azide. The mixture was stirred and warmed to 60° C. for 18 hr. After this time the mixture was cooled, poured into a 1 L separatory funnel containing 500 mL water and 250 mL of ethyl acetate. The pH was adjusted to 9.0 and the layers separated. The aqueous layer was extracted twice with 100 mL of ethyl acetate, the organic layers combined, dried over Na2SO4, filtered and concentrated to yield a product, which was carried to the next step without further purification.

1. customequipped with a condenser, magnetic stirrer, silicone oil heating bath, nitrogen inlet and gas outlet
2. temperatureAfter this time the mixture was cooled
3. additionpoured into a 1 L separatory funnel
4. customthe layers separated
5. extractionThe aqueous layer was extracted twice with 100 mL of ethyl acetate
6. dry with materialdried over Na2SO4
7. filtrationfiltered
8. concentrationconcentrated
9. customto yield a product, which
10. customwas carried to the next step without further purification