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Photolysis of 4-acetyl-4-ethoxyformylcyclohexanone, 4-acetyl-4-phenylcyclohexanoneand 1-acetyl-1-phenylcyclohexane in deuteriochloroform using a high pressure Hg-Xe lamp showedunusual polarizations. The results are explained by the formation of a singlet exciplex of the ketonewith deuteriochloroform and the photoaddition of deuteriochloroform to the ketone.