Structurally diverse aromatic aldehydes were thioacetalated in a clean and efficient reaction with ethane 1,2-dithiol and thiophenol based on the use of I2 generated in situ from Fe(NO3)3.9H2O/NaI. The reaction occurs in good to high yield in dichloromethane at room temperature and the use of toxic and corrosive molecular iodine is avoided.