Category: 41253-21-8

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

5-Fluoro-2-(lH-l,2,4-triazol-l~yl)benzonitrile. A suspension of 2,5- diflurobenzonitrile (4.5 g, 32.35 mmol) and 1,2,4-triazole sodium salt (3.6 g, 40 mmol) in dimethylformamide (40 mL) was heated at 80 0C for 15 h. The reaction mixture was then cooled, diluted with CH2Cl2 (200 mL), washed with water (3 X 30 mL) and brine (30 mL), then dried (Na2SO4), filtered and concentrated to give a white solid which was purified by flash column chromatography (SiO2) using 1 : 1 to 3:1 ethyl acetate/Hexanes to afford the title compound (2.98 g, 49% yield) as a white powder. 1H NMR (500 MHz, CDCl3) delta: 8.70 (IH, s), 8.18 (IH, s), 7.76 (IH, dd, J = 9.0, 4.8 Hz), 7.55 (IH, dd, J = 7.3, 2.8 Hz), 7.51-7.47 (IH, m). LCMS (M+H) calcd for C9H6FN4: 189.17; found: 189.10.

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; BRISTOL-MYERS SQUIBB COMPANY; WO2007/64316; (2007); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

41253-21-8, Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 41253-21-8, name is Sodium 1,2,4-triazol-1-ide, A new synthetic method of this compound is introduced below.

To a solution of phenol 11a (200 mg, 0.441 mmol) and cesium carbonate (158 mg, 0.485 mmol) in DMF (10 mL) was added 1,2-dibromoethane (96 muL, 1.11 mmol). The resulting mixture was stirred at room temperature for 60 h. After dilution with water, the mixture was extracted with EtOAc. The organic layer was dried over anhydrous MgSO4, filtered and concentrated in vacuo. The residue was carried on to the next step without further purification.To a solution of the crude bromide in DMF (10 mL) was added 1,2,4-triazole sodium derivative (122 mg, 1.34 mmol). The mixture was stirred at room temperature for 15 h. After dilution with water, the mixture was extracted with EtOAc. The organic layer was dried over anhydrous MgSO4, filtered and concentrated in vacuo. The residue was purified using RP preparative HPLC to provide the titled compound 11g (78 mg, 33%, 2 steps). 1H NMR (400 MHz, DMSO-d6) delta 8.59 (s, 1H), 8.02 (s, 1H), 7.95 (s, 1H), 7.77-7.71 (m, 1H), 7.47 (s, 1H), 7.13 (s, 1H), 6.78 (d, J = 3.2 Hz, 1H), 6.62-6.58 (m, 1H), 5.02-4.92 (m, 2H), 4.71-4.35 (m, 8H), 3.71-3.61 (m, 1H), 3.49-3.41 (m, 1H), 3.38-3.15 (m, 5H); MH+ 549.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Article; Lee, Suk Ho; Kim, Min Ju; Lee, Sung-Han; Kim, Jeongmin; Park, Hyun-Ju; Lee, Jinhwa; European Journal of Medicinal Chemistry; vol. 46; 7; (2011); p. 2662 – 2675;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

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. 41253-21-8

A mixture of 2,3-difluorobenzylnitrile (2.27 g, 16.3 mmol) and triazole sodium salt (1.33 g, 14.8 mmol) in tetrahydrofaran (5 mL) and dimethylformamide (10 mL) was stirred at 85 C. for 4 h. After concentration, the residue was purified by flash chromatography (SiO2) eluting with 25%-50% ethyl acetate/hexane. The isolated product was recrystallized from hot ethyl acetate/hexane to give the title compound as white needles (1.51 g, 54% yield). 1H-NMR (500 MHz, CDCl3) delta ppm: 8.50 (1H, d, J=2.4 Hz), 8.25 (1H, s), 7.69-7.67 (1H, m), 7.60-7.57 (2H, m). LCMS [M+H]+ calcd for C9H6N4F: 189.16; found: 189.14.

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 Sodium 1,2,4-triazol-1-ide.

Reference:
Patent; Bristol-Myers Squibb Company; US2007/111984; (2007); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

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

5-(2-Bromo-5-fluoro-phenyl)-1-methyl-2H-tetrazole. A mixture of 5-(2-bromo-5-fluoro-phenyl)-1H-tetrazole (1.0 g, 4.12 mmol), iodomethane (1.12 g, 10 mmol) and potassium carbonate (1.5 g) in dimethylformamide (5 mL) was stirred at room temperature for 16 hrs, then concentrated in vacuo. The residue was purified by column chromatography (SiO2, CH2Cl2) to provide 350 mg (Yield 33%) of the title compound as white crystals. 1H NMR (500 MHz, CDCl3) delta ppm: 4.00 (3H, s) 7.18-7.25 (2H, m) 7.72 (1H, dd, J=8.4, 5.0 Hz); 13C NMR (126 MHz, CDCl3) delta ppm: 34.59, 117.73, 119.58, 120.43, 127.57, 135.11, 153.43, 161.69. LC/MS m/z 257/259.

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; Bristol-Myers Squibb Company; US2007/129379; (2007); 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.

At room temperature, a four-necked bottle was charged with 120 g of acetonitrile, 1,2,4-triazole sodium salt (18.20 g, 0.2 mol), 2,4′-dichloroacetophenone (37.80 g, 0.2 mol) , heating to 80~85 C, heat preservation reaction 1-2h, the reaction is completed, the solvent is evaporated to dryness under reduced pressure, 50g of water is added, extracted with 150g of dichloromethane, washed with water, the solvent is dried, to obtain a white solid qualitative content of 98% The weight yield is 96%.

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; Huai’an Guorui Chemical Co., Ltd.; Wu Yaojun; Zhang Pu; Zhao Wei; Jin Yucun; Wang Fengyun; Chen Mingguang; Mao Gengsheng; (6 pag.)CN109535091; (2019); A;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

41253-21-8, Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 41253-21-8, name is Sodium 1,2,4-triazol-1-ide, This compound has unique chemical properties. The synthetic route is as follows.

Compound 271; Synthesis of N-(5-(lH-l.Z4-triazol-l-ylV2-f3A5-trimethoxybenzovn phenvPacetamide; As shown in Reaction 1, first, magnesium was added to l-bromo-3,4,5- trimethoxybenzene as a starting material. Then, Compound (VII) derivative was added thereto to obtain a compound [N-(5-fluoro-2-(3,4,5- trimethoxybenzoyl)phenyl)acetamide. Thus obtained compound [N-(5-fluoro-2- (3,4,5-trimethoxybenzoyl)phenyl)acetamide] (36.2mg, 0.1 mmol) was dissolved in DMF (2 ml), and 1,2,4-triazole-Na (28.5 mg) was added thereto at room temperature. The mixture was heated with stirring for 2 hours. After completion of the reaction, the reaction mixture was cooled to room temperature and diluted with an EtOAc solution. The organic layer was washed with water, and brine. The extracted organic layer was dried over anhydrous MgSO4, and the solid substance was filtered off. The remaining solvent was removed by vacuum evaporation. The resulting residue was purified by column chromatography (SiO2, n-Hex/EA=2/l?l/l) to obtain Compound 271 (25.6 mg, 65%).1H NMR (CDCl3) delta 10.812 (s, IH), 9.077 (s, IH), 8.788 (s, IH), 8.144 (s, IH), 7.767 (d, J = 8.36 Hz, IH), 7.564 (d, J = 8.52 Hz, IH), 6.956 (s, 2H), 3.954 (s, 3H), 3.879 (s, 6H), 2.264 (s, 3H). MS (ESI) m/z 397 (M+ + H).

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; CHONG KUN DANG PHARMACEUTICAL CORP.; WO2008/38955; (2008); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 41253-21-8, name is Sodium 1,2,4-triazol-1-ide, A new synthetic method of this compound 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¡Á20 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¡Á2 L of 2N aqueous hydrochloric acid solution and with 2¡Á8 L of water. The aqueous layer was separated and treated with 4¡Á10 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¡Á20 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.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

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

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

A suspension of 2,5-diflurobenzonitrile (4.5 g, 32.35 mmol) and 1,2,4-triazole sodium salt (3.6 g, 40 mmol) in dimethylformamide (40 mL) was heated at 80 C. for 15 h. The reaction mixture was then cooled, diluted with CH2Cl2 (200 mL), washed with water (3×30 mL) and brine (30 mL), then dried (Na2SO4), filtered and concentrated to give a white solid which was purified by flash column chromatography (SiO2) using 1:1 to 3:1 ethyl acetate/Hexanes to afford the title compound (2.98 g, 49% yield) as a white powder. 1H NMR (500 MHz, CDCl3) ?: 8.70 (1H, s), 8.18 (1H, s), 7.76 (1H, dd, J=9.0, 4.8 Hz), 7.55 (1H, dd, J=7.3, 2.8 Hz), 7.51-7.47 (1H, m). LCMS (M+H) calcd for C9H6FN4: 189.17; found: 189.10.

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, Sodium 1,2,4-triazol-1-ide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Naidu, B. Narasimhulu; Banville, Jacques; Beaulieu, Francis; Connolly, Timothy P.; Krystal, Mark R.; Matiskella, John D.; Ouellet, Carl; Plamondon, Serge; Remillard, Roger; Sorenson, Margaret E.; Ueda, Yasutsugu; Walker, Michael A.; US2005/267105; (2005); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Some common heterocyclic compound, 41253-21-8, name is Sodium 1,2,4-triazol-1-ide, molecular formula is C2H2N3Na, 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. 41253-21-8

To a solution of 2,4-difluorobenzonitrile (10 g, 72 mmol) dissolved in tetrahydrofuran (20 mL), and dimethylformamide (40 mL) was added the sodium salt of 1,2,4-triazole (6.3 g, 70 mmol) and the mixture was stirred at 90 C. for 3 h, filtered and concentrated. The residue was adsorbed onto Silica gel and purified by flash chromatography eluting with 0%-10%-30% ethylacetate/hexanes to give 4-fluoro-2-(1H-1,2,4-triazol-1-yl)benzonitrile as colorless needles (2.46 g, 18%) and 4-(1H-1,2,4-triazol-1-yl)-2-fluorobenzonitril as a white solid (0.746 g, 6%). 4-Fluoro-2-(1H-1,2,4-triazol-1-yl)benzonitrile. Colorless needles (2.46 g, 18% yield) 1H NMR (500 MHz, CDCl3) delta 8.89 (1H, s), 8.19 (1H, s), 7.85 (1H, dd, J=8.7, 5.6 Hz), 7.60 (1H, dd, J=8.8, 2.4 Hz), 7.28-7.24 (1H, m). LCMS (M+H) calcd for C9H6N4F: 189.05; found: 189.13. 4-(1H-1,2,4-Triazol-1-yl)-2-fluorobenzonitrile. White solid (0.746 g, 6% yield) 1H NMR (500 MHz, CDCl3) delta 8.66 (1H, s), 8.15 (1H, s), 7.79 (1H, dd, J=8.5, 6.7 Hz), 7.69 (1H, dd, J=9.5, 1.8 Hz), 7.65-7.63 (1H, m). LCMS (M+H) calcd for C9H6N4F: 189.05; found: 189.13.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 41253-21-8, its application will become more common.

Reference:
Patent; Bristol-Myers Squibb Company; US2007/111984; (2007); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

The chemical industry reduces the impact on the environment during synthesis 41253-21-8, name is Sodium 1,2,4-triazol-1-ide, I believe this compound will play a more active role in future production and life. 41253-21-8

Example 4 Selectivity in the Preparation of Intermediate III The procedure of Example 3 was repeated with various solvents and bases, and the reaction mixtures were analyzed using HPLC to determine the ratio of intermediate III to isomer IV impurity. Solvents used were acetonitrile (ACN), chloroform (CHCl3), dimethylformamide (DMF), dichloromethane (CH2Cl2), acetone, CH(OC2H5)2, N-methyl-2-pyrrolidone (MP), dimethylacetamide (DMA), methanol, water, toluene, and mixtures thereof. Bases used were sodium iodide (NaI), potassium t-butoxide (KOtB), potassium hydroxide (KOH), potassium carbonate (K2CO3), potassium iodide (KI), commercial sodium triazolate (NAT), tetrabutyl ammonium hydroxide (TBAI), and mixtures thereof. The results are summarized in Table 1 below, in which the units of dilution are parts by weight of solvent based on the weight of the 4-(bromomethyl)benzonitrile. As illustrated in Table 1, choice of solvent has the largest effect on the resulting ratio of intermediate III to isomer IV impurity. Choice of base, dilution, and reaction times/temperatures also affect the ratio of intermediate III to isomer IV impurity, but to a lesser degree. Dimethylacetamide solvent showed the most selectivity for intermediate III, followed by methylpyrrolidone.

The chemical industry reduces the impact on the environment during synthesis 41253-21-8. I believe this compound will play a more active role in future production and life.

Reference:
Patent; MacDonald, Peter Lindsay; Bigatti, Ettore; Rossetto, Pierluigi; Harel, Zvi; US2007/66831; (2007); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics