Application of 288-36-8, New Advances in Chemical Research in 2021. The transformation of simple hydrocarbons into more complex and valuable products via catalytic C–H bond functionalisation has revolutionised modern synthetic chemistry. 288-36-8, name is 1H-1,2,3-Triazole, molecular formula is C2H3N3, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, below Introduce a new synthetic route.
A suspension of NAOH (37.86 g, 946.5 mmol), sodium iodide (94.65 g, 631.5 mmol) and 1H- [1, 2, 3] triazole (61.03 g, 883.6 mmol) in 2-methyl-2-butanol (750 mL) was refluxed for 1 h under an inert atmosphere. After cooling to room temperature the methane sulfonate (94.18 g, 631.2 mmol) was added within 5 minutes. The resulting suspension was then heated to reflux for 3 h, cooled to room temperature and concentrated in vacuo at 45 C. Water (500 mL) and dichloro methane (1 L) were added and the organic phase was separated, dried over sodium sulfate and the volatiles removed at 30 C. The residue was distilled at 1 mmHg. A forerun was collected at 20-70 C. The main fraction distilled at 123-129C as a colourless, turbid liquid. After filtration over Celite 1- BUT-3-YNYL-IH- [1, 2,3] triazole was obtained as a colourless liquid (29.77 g, 38.9 %). ‘H-NMR (CDCL3) 8 : 2.05 (t, 1H), 2.75 (dt, 2H), 4.5 (t, 2H), 7.65 (s, 1H), 7.7 (s, 1H).
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Reference:
Patent; F. HOFFMANN-LA ROCHE AG; WO2004/96796; (2004); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics