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With trifluoroacetic anhydride In 1,4-dioxane; pyridine at -1.3 - 25℃; for 72 h; Inert atmosphere
In a 500 ml jacketed flask equipped with a mechanical stirrer, a temp probe, a circulation bath and a positive nitrogen atmosphere set up was placed with 1,2,4-triazole-3-carboxamide 25.3 gm (0.112 mole), 1,4-dioxane 225 gm, and pyridine 72.8 gm (0.92 mole). The mixture was chilled to -6.8° C. Trifluoroacetic anhydride 107.1 gm (0.51 mole) was added dropwise at -1.3 to -6.8° C. in 10 min. Then the mixture was warmed to ambient temperature and stirred for 30 min. Without work up, a sample was taken for HPLC analysis. The chromatogram showed that the product contained 93percent 3-CNT and 0.2percent 3-CAT.
Reference：
[1] Patent: US2009/292122, 2009, A1, . Location in patent: Page/Page column 12
[2] Bioorganic and Medicinal Chemistry Letters, 2018, vol. 28, # 1, p. 11 - 14
[3] Russian Journal of Bioorganic Chemistry, 2013, vol. 39, # 1, p. 53 - 71[4] Bioorganicheskaya Khimiya, 2013, vol. 39, # 1, p. 61 - 80,20
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