Pentaarylantimony Ar3Sb (Ar = Ph, p-Tol) arylates diarylbismuth arylsulfonates Ar2BiOSO2Ar' (Ar' = C6H4Me-4; C6H3Me2-2,4, C6H3Me2-2,5) in ether at 20 degreesC (48 h) to form triarylbismuth in yields of up to 95%. The second reaction product is tetraarylantimony arenesulfonate. The reaction of pentaphenylantimony with phenylbismuth bis(arenesulfonate) PhBi(OSO2Ar')(2) under the same conditions leads to formation of diphenylbismuth arenesulfonate and tetraphenylantimony arenesulfonate in yields of up to 90%.