反应详情

温度

100 °C

3-Bromo-benzonitrile 8a (18.2 g, 0.1 mol) and ammonium chloride (5.9 g, 0.11 mol) were dissolved in 80 mL of N,N′-dimethylformamide followed by addition of sodium azide (7.16 g, 0.11 mol) under argon atmosphere. The reaction mixture was heated to 100° C. and reacted overnight. Then the mixture was cooled to 60° C. and concentrated under reduced pressure to remove N,N′-dimethylformamide. The residue was diluted with 100 mL of water and 4 mL of concentrated hydrochloric acid and stirred for 1 hour. The mixture was filtered and dried to obtain the title compound 5-(3-bromo-phenyl)-1H-tetrazole 8b (23 g) as a white solid.

1. customreacted overnight
2. temperatureThen the mixture was cooled to 60° C.
3. concentrationconcentrated under reduced pressure
4. customto remove N,N′-dimethylformamide
5. additionThe residue was diluted with 100 mL of water and 4 mL of concentrated hydrochloric acid
6. filtrationThe mixture was filtered
7. customdried