The infrared (20 to 3100 cm<sup>−1</sup>) and Raman (10 to 3100 cm<sup>−1</sup>) spectra of gaseous (CH<sub>3</sub>)<sub>3</sub>SiOCH<sub>3</sub> and (CH<sub>3</sub>)<sub>3</sub>SiOCD<sub>3</sub> have been recorded. The Raman spectra of both liquids and the infrared and Raman spectra of the "light" compound in the solid state have also been recorded. A vibrational assignment based upon depolarization ratios, frequency shifts with isotopic substitution, and group frequencies is proposed. The Si—O torsional mode was observed at 67 cm<sup>−1</sup> which gives a barrier to internal rotation of 1.02 kcal/mol. Strong mixing of the Si—O—C bending mode with the C—Si—C bends is proposed. The CH<sub>3</sub>—O torsion was not observed.

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