Research speed reading 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
10.0 g of [COMPOUND 1] and 100 ml of tert-butyl acetate are loaded in a flask. The resulting suspension is kept under stirring at ambient temperature.8.30 g of N-bromosuccinimide (NBS) followed by 220 mg of catalyst azobisisobutyronitrile (AIBN) are then added. At this point, the resulting mixture is heated and kept at a temperature of 65-75C for 2-4 hours.The reaction quenching is performed by lowering first the temperature of the reaction mixture to 30-40C and then adding 50 ml of a 5% solution of sodium metabisulphite.At this point the organic rich phase is separated from thewater phase and then washed with distilled water.80 ml of dimethylformamide (DMF) are added to the rich solution, after the latter has been concentrated in a vacuum. The solution thus obtained is re-distilled to eliminate theresidual t-butylacetate solvent. 4.47 g sodium 1,2,4-triazole are added to the same solution, after the latter has been brought to a temperature of 0-25C (preferably 5-10C). The reaction mixture thus obtained is kept under stirring for 1-2 hours.The reaction is quenched by the addition of 100 ml toluene and 125 ml distilled water. After separation of the phases, the rich organic phase is treated with a. water solution HC1 0.lM.After separation of the phases, 1 g of carbon is added to the resulting organic phase and it is kept under stirring at ambient temperature.After filtering, the clarified organic phase is extractedtwice with 100 ml of HC1 2M. The rich water phase, containinghigh purity dissolved anastrozole, is lastly back-washed with toluene.Maintaining a temperature below 15C, a solution of NaOF{ at30 by weight is added to the rich acid solution in 60-90minutes until pH 1 is reached. The mixture is then left in crystallization break at 0-5C for 2 hours. A solution of NaOI-{ 0.5 M is then added until a pH of between 2.5 and 3.5 is obtained. The resulting suspension is then left in break at0-5C for a further 2 hours. A last quantity of NaOH 0.5 M solution is then added until a final pH of between 5 and 7 is reached, followed by a last break atThe product is lastly filtered, washed with distilled waterand then dried in a vacuum at a temperature of 50C.In this way 6.3-6.6 g of pharmaceutical grade anastrozole are obtained from 10 g of commercial grade ANA-3.In particular, the product has:anhydrous titre: 99.16% ÷ 101.10%; KF<0 .1%;total impurities: 0.21% ÷ 0.26%
The catalyzed pathway has a lower Ea, but the net change in energy that results from the reaction is not affected by the presence of a catalyst. In my other articles, you can also check out more blogs about 41253-21-8
Reference:
Patent; CORDEN PHARMA LATINA S.P.A. CON SOCIO UNICO; ANTONINI, Alberto; OLIVIERI, Lauso; SACCHITELLI, Doralinda; WO2014/184754; (2014); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics