Analyzing the synthesis route of Sodium 1,2,4-triazol-1-ide

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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

Now Is The Time For You To Know The Truth About Sodium 1,2,4-triazol-1-ide

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

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

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%].

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; 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

Introduction of a new synthetic route about 41253-21-8

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

Research speed reading in 2021. Redox catalysis has been broadly utilized in electrochemical synthesis due to its kinetic advantages over direct electrolysis. 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

EXAMPLE 1 A mixture of 2,2′-(5-methyl-1,3-phenylene)di(2-methylpropiononitrile), (2.26 g), N-bromosuccinimide (1.78 g), benzoyl peroxide (0.05 g) and carbon tetrachloride (50 ml) was heated under reflux for 2 h, cooled and filtered, and the filtrate was evaporated to dryness under reduced pressure. The residue was dissolved in dimethylformamide (20 ml), sodium triazole (1.8 g) was added, and the mixture was stirred at room temperature for 18 h. Water (100 ml) was added, and the mixture was extracted twice with ethyl acetate. The extracts were combined, dried and evaporated to dryness under reduced pressure, and the residue was purified by flash column chromatography, eluding with ethyl acetate, to give 2,2′-[5-(1H-1,2,4-triazol-1-ylmethyl)-1,3-phenylene]di(2-methylpropiononitrile), mp 81-82 after crystallisation from ethyl acetate/cyclohexane.

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; Imperial Chemical Industries plc; US4935437; (1990); A;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Research on new synthetic routes about 41253-21-8

This is the end of this tutorial post, and I hope it has helped your research about 41253-21-8!

Related Products of 41253-21-8, New Advances in Chemical Research in 2021. The transformation of simple hydrocarbons into more complex and valuable products via catalytic C–H bond functionalisation has revolutionised modern synthetic chemistry. 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, below Introduce a new synthetic route.

General procedure: 2-Chloro-N-(6-alkoxybenzo[d]thiazol-2-yl)acetamide (5 mmol) and sodium 1,2,4-triazole (6 mmol)were dissolved in N,N-dimethylformamide (10 mL) and stirred for 10 h at room temperature. Half of thesolvent was then evaporated, the solution was poured in 50 mL water, and extracted with ethyl acetate(30 mL 3). The ethyl acetate layer was dried over anhydrous MgSO4. After removing the solventunder reduced pressure, the crude product was obtained and recrystallized from dichloromethane toyield a white solid.

This is the end of this tutorial post, and I hope it has helped your research about 41253-21-8!

Reference:
Article; Liu, Da-Chuan; Zhang, Hong-Jian; Jin, Chun-Mei; Quan, Zhe-Shan; Molecules; vol. 21; 2; (2016);,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Simple exploration of Sodium 1,2,4-triazol-1-ide

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Related Products of 41253-21-8, New Advances in Chemical Research in 2021.Reactions catalyzed within inorganic and organic materials and at electrochemical interfaces commonly occur at high coverage and in condensed media, 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, below Introduce a new synthetic route.

To a solution of Intermediate 1d (12 mmol) in DMF (75 mL) was added the sodium salt of 1,2,4-triazole (5.5 g, 60 mmol). The resultant suspension was heated at 100-110 C. for 40 hr. After cooling the reaction mixture was poured into water (200 mL) and extracted with EtOAc (2200 mL). The combined extracts were washed with brine, dried over Na2SO4 and evaporated to afford a clear colorless oil. Chromatography through silica eluting with 2:3 hexanes/EtOAc furnished the BOC-protected amine as a clear colourless oil.

Therefore, this conceptually novel strategy might open impressive avenues to establish green and sustainable chemistry platforms.In my other articles, you can also check out more blogs about Sodium 1,2,4-triazol-1-ide.

Reference:
Patent; Merck & Co., Inc.; US6350760; (2002); B1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

The Shocking Revelation of 41253-21-8

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Related Products of 41253-21-8, New Advances in Chemical Research in 2021. The prevalence of solvent effects in heterogeneous catalysis in condensed media has motivated developing quantitative kinetic,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, below Introduce a new synthetic route.

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 salt (2.4 g, 27 mmol) were stirred in tetrahydrofuran (7 mL) and dimethylformamide (14 mL) at 95 0C 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) 6 ppm: 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.

I am very proud of our efforts over the past few months and hope to Sodium 1,2,4-triazol-1-ide help many people in the next few years.

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

Brief introduction of C2H2N3Na

The synthetic route of Sodium 1,2,4-triazol-1-ide has been constantly updated, and we look forward to future research findings.

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(4) Synthesis of 5-(4-chlorobenzyl)-2,2-bis-methoxymethoxymethyl-1-[1,2,4]triazol-1-ylmethylcyclopentanol (Compound (XXIV), G2=CH2OCH3, Ym=4-Cl, A=N)[1,2,4]-Triazole sodium salt (526 mg, 5.78 mmol) was dissolved in NMP (3 ml), and heated to an internal temperature of 115 degrees C. To this, 1 ml of a solution of 5-chlorobenzyl-2,2-bis-methoxymethoxymethyl-cyclopentanone (Compound No. (Compound (XXII), G2=CH2OCH3, Ym=4-Cl) 1.374g (3.85 mmol) in NMP was added. To this solution, sodium t-butoxide 333mg (3.47 mmol) and TMSOB 1.193 g (6.87 mmol) were added in portions while conducting the reaction at 115 degrees C for 5 hours. After completion of the reaction, the reaction solution was cooled to 35 degrees C, combined with 15 ml of water, and extracted with ethyl acetate. The organic layer was washed with water and saturated brine, dried over anhydrous sodium sulfate. The solvent was distilled away and the residue was subjected to silica gel column chromatography (eluent; ethyl acetate) for purification to obtain the desired substance. Product: 680.2 mgYield: 40.2 %Description: Colorless viscous liquid1H-NMR (CDCl3) delta:1.47-1.56 (1 H, m), 1.60-1.80 (2 H, m), 1.73-1.83 (1 H, m), 2.17 (1 H, dd, J = 13.2, 4.0 Hz), 2.22-2.31 (1 H, m), 2.44 (1 H, dd, J = 13.2, 10.3 Hz), 3.31 (3 H, s), 3.33 (1 H, d, J = 9.7 Hz), 3.38 (3 H, s), 3.46 (1 H, d, J = 9.7 Hz), 3.59 (2 H, s), 4.32 (1 H, d, J = 14.2 Hz), 4.41 (1 H, s), 4.45 (1 H, d, J = 6.4 Hz), 4.48 (1 H, d, J = 6.4 Hz), 4.54 (1 H, d, J = 14.2 Hz), 4.64 (2 H, s), 7.04 (2 H, d, J = 8.4 Hz), 7.21 (2 H, d, J = 8.4 Hz), 7.95 (1 H, s), 8.24 (1 H, s).

The synthetic route of Sodium 1,2,4-triazol-1-ide has been constantly updated, and we look forward to future research findings.

Reference:
Patent; KUREHA CORPORATION; ARAKI, Nobuyuki; YAMAZAKI, Toru; KUSANO, Nobuyuki; IMAI, Eiyu; KANNO, Hisashi; MORI, Masaru; MIYAKE, Taiji; WO2011/70771; (2011); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

The important role of C2H2N3Na

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To a solution of 2,4-difluorobenzonitrile (10 g, 72 mmol) dissolved in THF (20 mL), and DMF (40 mL) was added 1,2,4-triazole sodium derivative (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% EtOAc/hexanes to give intermediate 1 as colorless needles (2.46 g, 18%) and intermediate 2 was obtained as a white solid (0.7455 g, 6%). Intermediate 1 4-Fluoro-2-(1H-1,2,4-triazol-1-yl)benzonitrile: 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. Intermediate 2 4-(1H-1,2,4-triazol-1-yl)-2-fluorobenzonitrile: 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.

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; Bristol-Myers Squibb Company; US2007/112190; (2007); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Introduction of a new synthetic route about C2H2N3Na

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.

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. COA of Formula: C2H2N3Na

a stirrer after replacement with nitrogen,Add the thermometer and condenser to the reaction bottle1-(4-chlorophenyl)-4,4-dimethyl-3-butanone100g,Trimethyl thionyl chloride 63g,28 g of potassium hydroxide and 100 g of dimethyl sulfoxide (DMSO) and stirred.After 40 C reaction to 1 – (4 – chlorophenyl) – 4,4 – dimethyl -3 – pentanone reaction,Add sodium triazole sodium 60g, react at 120 C,After the reaction, desolvation, add 100 g of methylcyclohexane, and wash with 30 g of water.Layering at 70 C, recrystallization from water at 25 C,After suction filtration, the mixture was dried to obtain 130 g of tebuconazole, the yield was 91%, and the purity was 96%.

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; Jiangsu Qi Zhou Green Chemical Co., Ltd.; Wu Tianyu; Liu Yuchao; Tao Yachun; Cai Junyi; Wang Hai; (6 pag.)CN109336848; (2019); A;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

The important role of C2H2N3Na

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Sodium 1,2,4-triazol-1-ide, and friends who are interested can also refer to it.

Synthetic Route of 41253-21-8, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 41253-21-8 name is Sodium 1,2,4-triazol-1-ide, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

(2) Prepare a thermometer, a condenser,Add 250 ml of DMF and 1,2,4-triazole sodium salt (18.5 g 203 mmol) to a 250 ml four-neck reaction flask of a stirrer.Add 1-chloro-2-(4-chlorophenyl)-3-cyclopropylbutan-2-ol (44 g, 170 mmol),Heat to 100 C, reaction 60 ~ 100min, sample analysis,When the content of 1-chloro-2-(4-chlorophenyl)-3-cyclopropylbutan-2-ol is less than 1%,It is considered as the end of the reaction. Cool to room temperature,The reaction droplets were added to 120 ml of cold water.The precipitated solid was stirred, filtered, washed with water, dried.A cyproconazole having a content of 96% was obtained in a weight yield of 90%.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Sodium 1,2,4-triazol-1-ide, and friends who are interested can also refer to it.

Reference:
Patent; Huai’an Guorui Chemical Co., Ltd.; Zhang Pu; Li Ming; Jin Yucun; Chen Chao; Zhong Yu; Chen Mingguang; Wang Fengyun; (8 pag.)CN109400542; (2019); A;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics