反应详情

Sodium azide (6.0 g) was put in a 250 mL round-bottom flask (2-neck) equipped with a thermometer. H2O (20 mL) was added to dissolve sodium azide. It was cooled on an ice-water bath. A solution of 3-(perfluorooctyl)propionyl chloride (12.9 g) in acetone (25 mL) was added dropwise to keep the temperature below 12° C. The mixture was vigorously stirred for 2 h. Dimethyl ether (100 mL) and water (100 mL) are added, and the mixture was vigorously stirred for 1 min. After the separation of two layers, the aqueous layer was extracted with ether (2×50 mL). The ether layers were combined, and are washed with water (3×100 mL) and brine. After drying over MgSO4, the solvent was removed under vacuum to give a mixture of white solid and liquid (12.0 g) that was immediately used for the next reaction.

1. custom(2-neck) equipped with a thermometer
2. temperatureIt was cooled on an ice-water bath
3. customthe temperature below 12° C
4. stirringthe mixture was vigorously stirred for 1 min
5. customAfter the separation of two layers
6. extractionthe aqueous layer was extracted with ether (2×50 mL)
7. washare washed with water (3×100 mL) and brine
8. dry with materialAfter drying over MgSO4
9. customthe solvent was removed under vacuum
10. customto give
11. customwas immediately used for the next reaction