New discoveries in chemical research and development in 2021. The dynamic chemical diversity of the numerous elements, ions and molecules that constitute the basis of life provides wide challenges and opportunities for research. 41253-21-8, name is Sodium 1,2,4-triazol-1-ide belongs to triazoles compound, it is a common compound, a new synthetic route is introduced below. 41253-21-8
EXAMPLE 2; Preparation of 1,3-benezenediacetonitrile, alpha,alpha,alpha’,alpha’-tetramethyl-5-(1H-1,2,4-triazol-1-ylmethyl) (Formula I) 2 Kg of 2-[3-bromomethyl-5-cyano-dimethyl-methyl)-phenyl]-2-methyl-propionitrile and 10 L of N,N-dimethylacetamide were charged in a clean dry reactor followed by stirring for 10 minutes. 0.861 Kg of sodium triazole was charged under nitrogen pressure and the temperature raised to 57.5 C. The obtained solution was maintained for 36 hours at 57.5 C. and then cooled to about 25 C. followed by quenching the reaction by charging the solution to 30 L of water. The resultant reaction solution was extracted with 3×20 L of ethyl acetate followed by separation of organic and aqueous layers. The combined organic layer was distilled at 26.2 C. under a vacuum of -0.6 Kg/cm2 to afford a residue, the and the obtained residue was dissolved in 20 L of toluene followed by treatment with 2×2 L of 2N aqueous hydrochloric acid solution and with 2×8 L of water. The aqueous layer was separated and treated with 4×10 L of toluene and the obtained aqueous layer was charged into sodium bicarbonate solution, which was prepared by the dissolution of 4.7 Kg of sodium bicarbonate in 45 L of water. The obtained solution was stirred for 10 minutes and then extracted with 2×20 L of dichloromethane. A silica gel bed in a stainless steel column filter (2.05 cm diameter and 5.75 cm height) was prepared with 6.4 Kg of 230-400 mesh silica gel and the bed was washed with 4 L of ethyl acetate. The dichloromethane solution from above was passed through the silica gel bed and then the bed was washed with 38 L of ethyl acetate. The combined solution and washing was concentrated at 24.7 C. under a vacuum of -0.6 Kg/cm2 and cooled to 30 C. followed by dissolution of the residue in 1.4 L of isopropyl alcohol. The obtained solution was stirred for 10 minutes at 30 C. and 7 L of water were charged. The obtained suspension was stirred for 3 hours followed by filtration through a Nutsche filter and washing the obtained solid with a solution of 0.25 L of isopropyl alcohol and 1 L of water. The resultant solid was dried at 48 C. under vacuum of 690 mm Hg for 3 hours to afford 0.470 Kg of the title compound having a water content by Karl Fischer of 0.13% w/w.
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Reference:
Patent; Murki, Veerender; Palle, Venkata Raghavendra Acharyulu; Panchbhai, Pandurang Prasad; US2007/100148; (2007); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics