Ethyl thiooxamate → 6-Amino-3-(2-methyl-3-nitrophenyl)-1,2,4-triazin-5(4H)-one

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A mixture of 2-methyl-3-nitrobenzimidohydrazide (2.10 g, 10.81 mmol) and ethyl 2-amino-2-thioxoacetate (3.60 g, 27.0 mmol) in ethanol (100 mL) was heated at reflux for 8 hr, during which period product precipitated. Upon cooling to rt, the product, 6-amino-3-(2-methyl-3-nitrophenyl)-1,2,4-triazin-5(2H)-one (2.18 g) was collected as a white solid by suction filtration and dried under vacuum. This product was 88% pure by HPLC. It was used in the next step without further purification.

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