We introduce here a novel and simple method for the carbonylation of (alkoxyphenyl)diazirine. 3-(3-Methoxyphenyl)-3-trifluoromethyldiazirine was found to be stable under a typical Friedel-Crafts reaction producing carboxaldehyde derivatives of methoxyphenyldiazirine. The formyl group was easily converted to carboxylic acid, olefin, alcohol, or benzyl bromide providing new derivatives of diazirine photophor in the field of photoaffinity labeling.