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A thiazolyl azo dye 1-[(5-benzyl-1,3thiazol-2-yl)diazenyl]naphthalene-2-ol 233 has been synthesized from 2-amino-5-benzyl-1,3-thiazole 231 in an efficient synthetic procedure, involving Meerwein arylation, diazotization, and diazocoupling. Because compound 231 is a mild base, its efficient diazotization could be achieved only by using nitrososulfuric acid obtained from NaNO