Category: 41253-21-8

Synthetic Route of 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.

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) delta: 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.

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

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., Computed Properties of C2H2N3Na

10.0 g of the compound of formula (FF) as oil, as obtained according to ReferenceExample 1.1. 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 stirred 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 %.

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; SANDOZ AG; WILHELM, Thorsten; LANGNER, Martin; WO2012/172015; (2012); 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., category: Triazoles

This was made by displacing the 4-chloro phthalazine (Compound 195) with the sodium salt of 1,2, 4-triazole in DMF at55-65 C. BOCNH-P3 (L-tert-BuGly)-P2[(4R)-(4-(1, 2,4-triazo-1-yl) phthalazine-1-oxo)-S-proline]-Pl (1R,2S Vinyl Acca)-CONHSO2-Cyclopropane : the material was obtained as a white foam in 62% yield. LC/MSRt-min (MNa+) [method C]: 3.35 (774). 1H NMR (500 MHz, CD30D)8 ppm 0.97 (s, 9 H) 1. 01 (m, 2 H) 1.10 (s, 9 H) 1.16 (m,1 H) 1.37 (m, 2 H) 1.82 (m,1 H) 2.18 (d, J=8. 55 Hz,1 H) 2.32 (m,1 H) 2.69 (dd, J=13. 58,6. 87 Hz,1 H) 2.88 (br s,1 H) 4.06 (d,J=11. 60 Hz,1 H) 4.13 (s,1 H) 4.53 (m, J=9. 16 Hz,1 H) 4.61 (d,J=11. 90 Hz,1 H) 5.06 (d, J=10. 07 Hz,1 H) 5.23 (d,J=17. 40 Hz,1 H) 5.68 (m,1 H) 5.98 (s, 1 H) 7.97 (m, 2 H) 8.30 (m,J=11. 90 Hz, 2 H) 8.44 (d, J=7. 63 Hz,1 H) 9.14 (s, 1 H).

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; BRISTOL-MYERS SQUIBB COMPANY; WO2003/99274; (2003); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Application of 41253-21-8,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.

Intermediate 46′ 2-(lH-l,2,4-triazol-l-yl)benzonitrile: A suspension of 2-fluorobenzylnitrile(3.0 g, 25 mmol) and 1,2,4-triazole sodium complex (2.4 g, 27 mmol) were stirred in THF (7 mL) and DMF (14 mL) at 95 C for 18 h. After cooling and concentrating, the product was crystallized from hot CH2Cl2/hexane (1:1) to give the title compound as a white solid (4.25 g, 100% yield). 1H-NMR (300 MHz, CDCl3) delta: 8.74 (IH, s), 8.16 (IH, s), 7.82 (IH, dd, J= 4.9,1.3 Hz), 7.77-7.25 (2H, m), 7.57-7.51 (IH, m). LCMS [M+H]+ calcd for C9H7N4: 171.06; found: 171.12.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Sodium 1,2,4-triazol-1-ide, its application will become more common.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; WO2007/58646; (2007); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 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. Application In Synthesis of Sodium 1,2,4-triazol-1-ide

First, 3.8 g of 1,2,4-triazole were dissolved in 8 ml of NMP at 2O0C. Then,2.2 g of NaOH and 22 ml of NMP were added in portions over 1 hour, maintaining the temperature at less than 350C. The solution was stirred for 2 hours at 20C, and 7.8 g of Na2SO4 were then added. After filtration of the solid, the resulting solution was transferred to a dropping funnel, and added over 75 minutes to a solution of 14 g of crude l,3-benzenediacetonitrile-5-(bromomethyl)-alpha,alpha,alpha’,alpha’ tetramethyl (having a purity of 81.8%, containing: 3,5-bis(2-cyanoisopropyl)toluene 4.0%, l,l-dibromo-3,5-bis(2- cyanoisopropyl)toluene 10.7%, and other impurities 3.5% ) in 20 ml of NMP, cooled to -3O0C. At the end of the addition, the suspension was stirred at -300C for 18 hours, and monitored via HPLC. When the concentration of starting material is less than 0.5 percent, an amount of acetic acid sufficient to give a pH of about 6.5 to about 7.0 is added (an HPLC analysis of the crude reaction mixture showed: residual starting material 0.4%, Anastrozole 68.9%, Isoanastrozole 5.5%, 3,5-bis (2-cyanoisopropyl)toluene 7.5%, 1,1-dibromomethyl- 3,5-bis(2-cyanoisopropyl)benzene, and 15.4%, and other impurities 2.3%.). The mixture is then allowed to warm slowly to 200C, filtered, and 37 ml of toluene, 75 ml of heptane, and 37 ml of water are added. The biphasic system is stirred vigorously for 30 minutes, and the organic layer is then separated. Water, toluene, and heptane in amounts of 25 ml, 25 ml, and 50 ml, respectively, are added to the aqueous phase, and the system is stirred for 30 minutes before the organic phase is separated. Then, 10 ml of toluene and 20 ml of heptane are added to the aqueous phase, and the system is stirred for 30 minutes before the organic phase is separated. Toluene and water, 99 ml and 400 ml, respectively, are added to the aqueous phase, and the resulting biphasic system is stirred for 1 hour. The organic layer is separated and washed 3 times with a mixture of MeOH and water (3 ml and 21 ml, respectively). The final organic phase is concentrated to 45 ml under reduced pressure at 400C, and 45 ml of heptane are added dropwise over 1 hour. The resulting suspension is cooled to 00C, stirred for 1 hour, and filtered. The crude solid is dissolved in toluene (40 ml) at 4O0C, and heptane (40 ml) is slowly added under stirring. The suspension is cooled to 00C, stirred for 1 hour, EPO and filtered. The solid is driejd at 55C under reduced pressure until constant weight is achieved, yielding 5.8 g of product with a purity as follows: Anastrozole 98.45%, Isoanastrozole 0.09%, 3,5-bis (2-cyanoisopropyl)toluene 0.06%, l-bromo-3,5-bis (2- cyanoisopropyl)toluene 0.11%, l,l-dibromo-3,5-bis(2-cyanoisopropyl)toluene 0.07%, other impurities 1.22% are by HPLC.

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

Reference:
Patent; SICOR, INC.; WO2006/108155; (2006); A2;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Electric Literature of 41253-21-8, 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.

in a 2000 L finished synthesis kettle, 138 kg of sodium triazole sodium salt was dissolved in 15 kg of formamide. Adding N,N-dimethylformamide mother liquor, slowly raising the temperature to 80 C at a rate of 55 C / h, and reacting at 80 C for 8 hours, Then, N,N-dimethylformamide was recovered under a vacuum of -0.085 MPa for 2.7 hours. After the completion of the collection, the mixture is transferred to a high-vacuum distillation still for fractional distillation, and the mixture is fractionated under a vacuum of 1.33 kPa and a temperature of 227 C for 8 hours, and cooled to room temperature to obtain a fluorosilazole; wherein, the formula of the specific alkylation reaction is as follows: Formula (3).

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; Shanxi Hengrun Chemical Co., Ltd.; Fan Ming; Li Cangzhen; Chen Dunguo; Chao Liumin; Wang Jianqiao; Yin Weixin; (7 pag.)CN108864165; (2018); A;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Synthetic Route of 41253-21-8,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.

To 1.5 kg of crude alpha,alpha,alpha’,alpha’-tetramethyl-5-bromomethyl-1,3-benzene-diacetonitrile 5 (purity >80%, about 3 mol) in 7.5 l_DMF 0.275 kg 1,2,4-triazole sodium (3 mol) were added. The mixture was stirred at room temperature for 1 hr. After completion, 10 l ethyl acetate and 25 l water were added. The mixture was stirred for about 10 minutes and then phase separated. To the aqueous layer 5 l ethyl acetate were added. The mixture was stirred for about 10 minutes and then phase separated. The aqueous layer was discarded, and the organic layers were combined. The combined organic layers were washed with 10 l water twice. The organic layer was concentrated to dryness to obtain the crude anastrozole 6 (90%, purity>60%). The crude product was purified by flash column chromatography (silica) using ethyl acetate as eluent (purity>98%). Finally, the pre-purified anastrozole was re-crystallised from ethyl acetate/cyclohexane (1:2) to obtain 6 with a purity of more than 99.9%. Yield 34%.

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

Reference:
Patent; HELM AG; US2006/217569; (2006); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Related Products of 41253-21-8,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.

5-Fluoro-2-(1H-1,2,4-triazol-1-yl)benzonitrile. A suspension of 2,5-difluorobenzonitrile (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¡Á30 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 (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.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Sodium 1,2,4-triazol-1-ide, its application will become more common.

Reference:
Patent; Bristol-Myers Squibb Company; US2007/129379; (2007); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Electric Literature of 41253-21-8,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.

Ethyl chloroformate (13g) was slowly added dropwise to the solvent of triazole sodium salt (9.1g) in tetrahydrofuran (30mL) at 20-30 C, and the reaction was completed at 20-30 C for 1h. After the reaction is completed, filter to obtain a solution of ethyl 1,2,4-triazole-1-carboxylate in tetrahydrofuran; from -40 to -30, slowly add a solution of ethyl 1,2,4-triazole-1-carboxylate in tetrahydrofuran. A solution of LDA (lithium diisopropylamide) in tetrahydrofuran (2M, 60mL) was added dropwise. After reaction for 30min, ethyl chloroformate (13g) was added dropwise. After stirring for 30min, the temperature was slowly raised to 20-30 C and stirred for 2h; After completion, add 30% aqueous sodium hydroxide solution to the system and react at 80 90 for 2h. After completion of the reaction, cool to 0 10 , add hydrochloric acid to adjust pH 2 3, and filter to obtain 1, 2, 4-triazole -3-carboxylic acid, yield 82%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Sodium 1,2,4-triazol-1-ide, its application will become more common.

Reference:
Patent; Shanghai Dongyue Pharmaceutical Co., Ltd.; An Na; Liu Xinke; Long Zhongzhu; Cai Chang; Cai Shuihong; (5 pag.)CN110903255; (2020); A;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 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. Product Details of 41253-21-8

1.4: tert-butyl 4-cyclohexyl-4-(1H-1,2,4-triazol-1-ylmethyl)piperidine-1-carboxylate 7.83 g of tert-butyl 4-cyclohexyl-4-{[(methylsulphonyl)oxy]methyl}-piperidine-1-carboxylate and 5.68 g of sodium 1,2,4-triazole are introduced into a 100 ml round-bottomed flask under N2. 42 ml of dimethylformamide are added. After reaction in a microwave at 150 C. for 1 h 30 min and with a power of 150 W, the product is hydrolyzed and extracted with ethyl acetate until the aqueous phase is completely depleted. The organic phase is washed with H2O and concentrated to dryness. After crystallization from hexane, 4.42 g of tert-butyl 4-cyclohexyl-4-(1H-1,2,4-triazol-1-ylmethyl)piperidine-1-carboxylate are obtained. 1.5: 4-cyclohexyl-4-(1H-1,2,4-triazol-1-yl-methyl)piperidine 11.2 g of tert-butyl 4-cyclohexyl-4-(1H-1,2,4-triazol-1-ylmethyl)-piperidine-1-carboxylate are placed in 80 ml of 4N hydrochloric acid in dioxane. The reaction medium is stirred for 16 h at ambient temperature. After evaporation to dryness, the precipitate obtained is filter-dried and rinsed with diethyl ether. The hydrochloride thus obtained is dried over P2O5 under reduced pressure. 9.65 g of 4-cyclo-hexyl-4-(1H-1,2,4-triazol-1-ylmethyl)piperidine are obtained.

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

Reference:
Patent; SANOFI-AVENTIS; US2007/149562; (2007); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics