New discoveries in chemical research and development in 2021. Chemo-enzymatic cascade processes are invaluable due to their ability to rapidly construct high-value products from available feedstock chemicals in a one-pot relay manner. 49607-51-4, name is 1-Methyl-1H-1,2,4-triazol-3-amine belongs to triazoles compound, it is a common compound, a new synthetic route is introduced below. HPLC of Formula: C3H6N4
3,4-Dimethylfuran-2,5-dione (550 mg, 4.36 mmol, 1.05 equiv) and 1-methyl-1H-1,2,4-triazole-3-amine (407 mg, 4.15 mmol, 1.00 equiv) were dissolved in concentrated acetic acid (15 ml) and stirred under reflux conditions for 7 h. After cooling to room temperature, water and ethyl acetate were added and the mixture was extracted. The aqueous phase was repeatedly re-extracted vigorously with ethyl acetate, and the combined organic phases were then dried over magnesium sulfate, filtered and concentrated. Final purification by column chromatography of the resulting crude product (gradient ethyl acetate/heptane) gave 3,4-dimethyl 1-(1-methyl-1H-1,2,4-triazol-3-yl)-1H-pyrrole-2,5-dione in the form of a colorless solid (90 mg, 10% of theory). 1H-NMR (400 MHz, d6-DMSO delta, ppm) 8.09 (s, 1H), 3.75 (s, 3H), 2.01 (s, 6H).
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Reference:
Patent; Bayer CropScience Aktiengesellschaft; Bayer Aktiengesellschaft; FRACKENPOHL, Jens; HELMKE, Hendrik; FRANKE, Jana; REINGRUBER, Anna Maria; MACHETTIRA, Anu Bheemaiah; GATZWEILER, Elmar; ROSINGER, Christopher Hugh; SCHMUTZLER, Dirk; DIETRICH, Hansjoerg; LUEMMEN, Peter; (96 pag.)US2019/330192; (2019); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics