PURPOSE:To recover the title compound of high purity in high yield, said compound which is used as a basic material for silicone oil by allowing aqueous ammonia to react with a mixed solution of ethyl acetate, hexamethyl disiloxane, separating into the organic layer and the aqueous layer and treating the organic layer. CONSTITUTION:An organic mixed solution mainly containing ethyl acetate and hexamethyl disiloxane is combined with aqueous ammonia to effect the reaction with each other under stirring at room temperature of about 25 deg.C to convert ethyl acetate into acetamide and ethanol. These products shift into the aqueous phase, because they are soluble in water. The organic phase is separated from the aqueous phase and the subject hexamethyl disiloxane is collected from the organic phase.
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