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0 °C

A solution of 1-phenyl-5-tetrazolone (30 g) in acetonitrile (300 mL) was stirred under argon at 0° C. and nitronium tetrafluoroborate (36.9 g) was added over 30 minutes. After stirring at 0° C. for an additional 30 minutes the mixture was poured into water (900 mL). The precipitate was collected by filtration and dried under vacuum to give 23.1 g of the title compound as cream-colored solids. The filtrate was extracted with ethyl acetate, dried (MgSO4), filtered, and concentrated to give an additional 8.6 g of solids which was a 1:1 mixture of ortho- and para-substituted isomers. 1H NMR (acetone-d6) δ 13.62 (br s, 1H), 8.36 (ABq, JAB=9.2 Hz, 4H); MS (EI) m/z 207 (M+); Rf=0.2 (10% methanol/dichloromethane).

1. filtrationThe precipitate was collected by filtration
2. customdried under vacuum