From quinquenary organobismuth compounds

To a solution of pentaphenylbismuth (3 g, 5 mmol) in dry benzene (8 ml) under an argon atmosphere, a solution of trifluoromethanesulfonic acid (0.750 g, 5 mmol) in ether (10 ml) was added dropwise with stirring under water cooling at 15°C. Addition was continued until complete decolorization had occurred. After subsequent addition of ether, the white solid formed was filtered off, washed with cold ether, and dried in vacuo to obtain the bismutho-nium trifluoromethanesulfonate (2.9 g, 90%), m.p. 205-215°C (hexane-dichloromethane) [85JCS(P1)2657]. 

To a suspension of pentaphenylbismuth (1.6 g, 2.7 mmol) in anhydrous ether (10 ml) was added triphenylborane (0.7g, 3 mmol) in anhydrous benzene (10 ml) under a nitrogen atmosphere. The white crystals immediately precipitated were crystallized twice from nitromethane to obtain the bismuthonium tetraphenylborate as colorless needles (1.1 g, 49%), m.p. 225-228°C [52LA(578)136]. 

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