Nuclear methylation of phloracetophenone and 3-C-methyl phloracetophenone, under vigorous conditions yields 5-acetyl-1∶1∶3∶3-tetramethyl cyclohexen-(4)-ol-(4)-dione (2∶6) (III); the intermediate 3∶5-dimethyl compound could not be obtained. This method is convenient for the preparation of leptospermone (VI). Many natural products seem to be formed by the nuclear methylation of the carbonyl derivatives of phloroglucinol. Using lesser proportions of alcoholic potash lower methylation products are obtained; but 3∶5-dimethyl-phloroacetophenone could be isolated only in small quantities.