Nitration of di-n-butyl benzylphosphonate, with fuming nitric acid or with mixed acid, was now found to give good yields of the p-nitro derivative. Other isomers, of which the ortho might have been expected, were formed in such small amounts as to avoid detection. The preparation of a p-nitrobenzylphosphonate is of interest because of the reported failure of an attempted direct preparation from trialkyl phosphites and 9-nitrobenzyl chloride.