Abstract
Objectives: To improve and scale up the synthesis of 5-amino-2-methylbenzenesulfonamide (2) to achieve a yield of 200 g/batch from p-nitrotoluene. Methods: Utilizing reaction techniques including reductive acylation, chlorosulfonation-amidation, hydrolysis; thin-layer chromatography; measuring melting point and spectroscopic tools such as infrared (IR), mass spectrometry (MS), and nuclear magnetic resonance (1H-NMR and 13C-NMR). Results: The synthesis of 5-amino-2- methylbenzenesulfonamide (2) from p-nitrotoluene has been improved in three stages at a scale of 200 g/batch, with an overall process yield of 58.4%, higher than the reported literature. The technical improvements include avoiding the use of toxic solvents such as methanol and acetone, developing a secure loading procedure, and enhancing product puri¦cation conditions to boost productivity.
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