Abstract Procedures have been developed for the acylation of 4-amino-4'-nitrodiphenyl sulfide with an almost quantitative yield by the action of acetic anhydride in aprotic organic solvents and subsequent nitration of 4-acetylamino-4'-nitrodiphenyl sulfide with nitric acid in a mixture of acetic acid and an aprotic organic solvent with addition of a mixture of sulfuric and acetic acids by the end of the process.