Carbonyl compounds are conveniently converted into their corresponding dimethyl acetals in good yields and short reaction times by means of a photochemical reaction in methanol with a catalytic amount of chloranil (2, 3, 5, 6-tetrachloro-1, 4-benzoquinone, CA) as the sensitizer. Using aldehydes gives better results than using ketones, which also tend to form enol ethers as side products. These results are similar to those of simple acid-catalyzed ...