Category: 41253-21-8

A common compound: 41253-21-8, name is Sodium 1,2,4-triazol-1-ide, belongs to Triazoles compound, it can change the direction of chemical reaction, and react with certain compounds to generate new functional products. A new synthetic method of this compound 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% ¡Â 101.10%; KF<0 .1%;total impurities: 0.21% ¡Â 0.26% In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 41253-21-8, other downstream synthetic routes, hurry up and to see. 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

41253-21-8, Adding some certain compound to certain chemical reactions, such as: 41253-21-8, name is Sodium 1,2,4-triazol-1-ide, 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 41253-21-8.

(Exl.f) Preparation of the compound of formula (GG)10.0 g of the compound of formula (FF) as oil, as obtained according to (Exl .e), were dissolved in 80 ml of DMSO under stirring. Then, 10 g of the sodium salt of 1,2,4-triazole were added at 25 to 30 C, and the resulting reaction mixture was stirred for 24 hours at 85 to 90 C. The mixture was then cooled to 25 to 30 C, and 25 ml of 5 % (w/v) aqueous solution of sodium hydroxide were added. The mixture was then stin-ed for 3 hours at 25 to 30 C. 100 ml of water were added, and the product was extracted into 150 ml of methyl tetrahydrofuran. The thus obtained organic layer was washed with a 10 % (w/v) aqueous solution of sodium chloride, and subsequently the solvents of the resulting separated organic layer were removed by distillation under reduced pressure to obtain the title compound of formula (GG)as a crude oil. The yield was 6.0 g, corresponding to a theoretical value of 86.0 %.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 41253-21-8.

Reference:
Patent; SANDOZ AG; OBERHUBER, Michael; SALCHENEGGER, Joerg; DE SOUZA, Dominic; ALBERT, Martin; WILHELM, Thorsten; LANGNER, Martin; STURM, Hubert; SPITZENSTAeTTER, Hans-Peter; WO2011/144653; (2011); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

41253-21-8, A common heterocyclic compound, 41253-21-8, name is Sodium 1,2,4-triazol-1-ide, molecular formula is C2H2N3Na, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Preparation of 4-cyclohexyl-4-[1,2,4]triazol-1-ylmethyl-piperidine-1-carboxylic acid tert-butyl ester (5): To a solution of 4-cyclohexyl-4-methansulfonyloxymethyl-piperidine-1-carboxylic acid tert-butyl ester (39 g, 103.8 mmol) in N,N-dimethylformamide (200 mL) is added sodium triazole (38 g, 415.2 mmol). The resulting solution is heated to 100 C. for 24 hours then cooled to room temperature. The solvent is removed under reduce pressure and the crude product purified over silica (80:20 EtOAc:hexane) to afford 28.7 g (79.7% yield) of the desired compound as a colorless solid. 1H NMR (CD3OD) delta0.95-1.90 (m, 15H), 1.46 (s, 9H), 3.45-3.55 (m, 4H), 4.34 (s, 2H), 7.99 (s, 1H), 8.48 (s, 1H). MS (ESI) m/z 349, (M+H+), 371(M+Na+)

The synthetic route of 41253-21-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Ebetino, Frank Hallock; Liu, Xuewei; Solinsky, Mark Gregory; Wos, John August; Mumin, Rashid Naeem; US2004/10010; (2004); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 41253-21-8 as follows. 41253-21-8

e) Preparation of 2,2′-[5-(1H-1,2,4-triazole-1-yl-methyl)-1,3-phenylene]di(2-methyl propionitrile) (1)A mixture of 2,2′-(5-bromomethyl-1,3-phenylene)di(2-methylpropionitrile) (V) (4 gm, 0.013 moles) and 1,2,4-triazole sodium salt (2.40 gm, 0.026 moles) in N,N-dimethylformamide (28 ml) was heated under stirring at 45-50 C. for 4 hour. The reaction mixture was cooled, poured into the ice-water and extracted with ethyl acetate. The ethyl acetate layer was separated and concentrated to give a residue. This residue was diluted with water, acidified with concentrated hydrochloric acid (adjusted the pH tol-2). The reaction mixture was heated at 50 C. and subsequently filtered the hot solution. The mother liquor was treated with ammonia solution at 0-5 C. (adjusted the pH to 8-9) and extracted with ethyl acetate. The ethyl acetate layer was separated and concentrated to obtain a residue (3.0 g).f) Purification of Anastrozole by Column Chromatography and CrystallizationThis residue was purified through column chromatography by using silica gel column and ethylacetate-hexane (740 ml: 950 ml) as eluent. The solid (2.0 g) obtained was recrystallized using a mixture of acetone-water (12 ml: 20 ml) or ethylacetate-hexane mixture (9 ml to 18 ml) to obtain 2,2′-[5-(1H-1,2,4-triazole-1-ylmethyl)-1,3-phenylene]di(2-methyl propionitrile) (1). [Yield: 34.0%, purity, 99.9%].

According to the analysis of related databases, 41253-21-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Radhakrishnan, Tarur Venkatasubramanian; Baban, Bhise Nandu; Govind, Sathe Dhananjay; Janardan, Chaudhari Chhayendra; Ashokkumar, Joshi Mehul; US2008/207915; (2008); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics