反应详情

5-(2′-Methoxy-biphenyl-3-yl)-1H-tetrazole 8c (15.5 g, 61.5 mol) was dissolved in 195 mL of acetic acid followed by addition of 195 mL of hydrobromic acid under argon atmosphere. The reaction mixture was heated to reflux for 5 hours. The reaction was monitored by TLC until the disappearance of the starting materials. The mixture was cooled to room temperature overnight. The mixture was filtered and the filter cake was dissolved in 500 mL of ethyl acetate. The mixture was washed with water (500 mL×2), dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure. The residue was recrystallized from 100 mL of ethyl acetate to obtain the title compound 3′-(1H-tetrazol-5-yl)-biphenyl-2-ol 8d (12 g, yield 82.8%) as a white solid.

1. temperatureThe reaction mixture was heated
2. temperatureto reflux for 5 hours
3. filtrationThe mixture was filtered
4. dissolutionthe filter cake was dissolved in 500 mL of ethyl acetate
5. washThe mixture was washed with water (500 mL×2)
6. dry with materialdried over anhydrous sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure
9. customThe residue was recrystallized from 100 mL of ethyl acetate