Extracurricular laboratory: Synthetic route of 98-97-5

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Adding a certain compound to certain chemical reactions, such as: 98-97-5, name is Pyrazine-2-carboxylic acid, belongs to Pyrazines compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 98-97-5, name: Pyrazine-2-carboxylic acid

To a solution of Pyrazine-2-carboxylic acid (295mg, 2. [1MMOL,] leq) and triethylamine [(765UL,] 5.4mmol, 2.6eq) in THF (6ml) at [0 C] was added dropwise diphenylphophoryl azide [(L.] 4ml, 2. [8MMOL,] [1.] 3eq). The mixture was stirred under nitrogen at [0 C] for 30 minutes, then warmed to RT and stirring continued for a further 2 hours. The reaction mixture was concentrated under vacuum and purified by flash chromatography [(90/10-60/40] [ISO-HEXANE/ETOAC)] to afford the title compound as white solid (265mg, yield=78%). 1H NMR (400 MHz, [CDC13)] [6] 9.14 (d, 1H, J=1.2) ; 8.50 (dt, 1H, J=1.2, 0.4), 2.62 (s, 3H, broad).

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Reference:
Patent; MILLENIUM PHARMACEUTICALS, INC.; WO2003/101444; (2003); A1;,
Pyrazine – Wikipedia,
Pyrazine | C4H4N2 – PubChem