PURPOSE:To recover the titled compound useful as a silylating agent in medical industry, etc., by utilizing tert-butyldimethylsilanol as a waste, by reacting tert-butyldimethylsilanol with phosphorus chloride. CONSTITUTION:tert-Butyldimethylsilanol formed from tert- butyldimethylchlorosilane after use as a silylating agent is reacted with a phosphorus chloride (example; phosphorus trichloride, phosphorus pentachloride, phosphorus oxychloride, etc.) preferably at 1:1-1.2 molar ratio, as necessary in the presence of a chlorinated hydrocarbon solvent and transformed into the aimed compound, which is recovered.
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