The development of a safe and practical process for the potassium and sodium salts of 3-Methyl-4H-[1,2,4]oxadiazol-5-one 1A and 1B is described. The focus of the report is how the scale-up issues of the original procedure are overcome, in particular, the thermal hazards of the starting material, hydroxylamine, and the intermediate, acetamidoxime 4. The final process was demonstrated multiple times on a 600-L scale with consistent yields (70%) and purities (95%).
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