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According to a preferred process of the present invention, hexamethyl disiloxane (HMDO) is separated from a mixture of HMDO and toluene by using pyrrolidine as an azeotrope former for the HMDO. For spent solvent containing essentially 91% by weight toluene, 8% by weight HMDO, and 1% by weight water, the solvent is first dehydrated with a suitable drying agent such as calcium oxide, sodium sulfate,
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