A novel one-pot approach for the preparation of 2-mercaptobenzaldehyde, 2-mercaptocyclohex-l-enecarboxal- dehydes and 3-mercaptoacrylaldehydes [（Z）-3-mercapto-2-methyl-3-phenylacrylaldehyde, 3-mercapto-3-（o-tolyl）- acrylaldehyde）] starting from ortho-bromobenzaldehyde, 2-chlorocyclohex-l-enecarbaldehydes, （Z）-3-chloro-2- methyl-3-phenylacrylaldehyde and 3-chloro-3-（o-tolyl）acrylaldehyde is reported. The reaction of sulfur with the Grignard reagent of the acetal for the protection of the aldehyde group affords the title compounds through hydroly- sis with dilute hydrochloric acid in high yields.
