Analysis of the infrared spectra of some polydeuterated toluenes obtained by proton exchange with BF<sub>3</sub>–D<sub>3</sub>PO<sub>4</sub> demonstrated the unreliability of this analytical tool in the 4000–900 cm<sup>−1</sup> region. Useful correlations can be obtained in the 900–500 cm<sup>−1</sup> region if suitable instrumentation is available. The previously unreported spectra of toluene-2,5-D, and toluene-3,5-D and toluene-2,4,6-D are described.
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