Category: 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. HPLC of Formula: C2H2N3Na

150 g (1 eq) of compound G was added to 1.5 L of DMF and added178 mg (5 eq) of sodium triazole and 38 ml of 1,3-dimethylpropylene urea (DMPU),And the mixture was stirred at 100 to 110 C for 24 hours.The reaction mixture was cooled to room temperature, 1.5 L of water was added to the reaction solution, and impurities were extracted with 400 ml of * 2 DCM. The organic phase was washed with 300 ml of 6NHCl extraction, hydrochloric acid aqueous solution with 100ml * 2DCM washing, separation of hydrochloric acid aqueous solution, temperature control below 30 50% NaOH adjusted PH = 8-9, extracted with 500ml * 2EA, combined EA, 300ml * 5 washing, 300mlBrine, brine, dried over Na2SO4 and concentrated to give a yellow oil. 200 ml of EA was added,Solution, dropping 800ml n-heptane solid wash, stirring at room temperature 3h, suction filtration, 200ml n-heptane washing, wasTo a white solid compound H of 86.9 g, Y = 68.5%, pur = 95.2%.

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; Chongqing Weipeng Pharmaceutical Co., Ltd; Han, Gongchao; Zhou, Zhiliang; Zhou, Xingguo; Xiang, Yong; Xiang, Linling; Gong, Xue; (8 pag.)CN105440022; (2016); A;,
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. Recommanded Product: Sodium 1,2,4-triazol-1-ide

10.0 g of the compound of formula (FF) as oil, as obtained according to Reference Example 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%.

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; SANDOZ AG; Wilhelm, Thorsten; Langner, Martin; US2014/303184; (2014); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

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.

Compound 271Synthesis of N-(5-(1H-1,2,4-triazol-1-yl)-2-(3,4,5-trimethoxybenzoyl)phenyl)acetamide; As shown in Reaction 1, first, magnesium was added to 1-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] (36.2 mg, 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=2/1?1/1) to obtain Compound 271 (25.6 mg, 65%).1H NMR (CDCl3) delta 10.812 (s, 1H), 9.077 (s, 1H), 8.788 (s, 1H), 8.144 (s, 1H), 7.767 (d, J=8.36 Hz, 1H), 7.564 (d, J=8.52 Hz, 1H), 6.956 (s, 2H), 3.954 (s, 3H), 3.879 (s, 6H), 2.264 (s, 3H). MS (ESI) m/z 397 (M++H).

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; CHONG KUN DANG PHARMACEUTICAL CORP.; US2009/275575; (2009); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Related Products of 41253-21-8, These common heterocyclic compound, 41253-21-8, name is Sodium 1,2,4-triazol-1-ide, 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.

The 2mmol 3b dissolved in 10mLDMF, to the reaction solution was added 10mmol triazole sodium salt compound 4 and 2mmol DMPU, heated to 100-110 C and stirred for 24 hours. The mixture was quenched with water (1.5 L) and extracted with dichloromethane (50 mL * 2). The dichloromethane phase was washed once with saturated brine (20 mL), dried over Na2SO4 and concentrated to give a yellow oil which was purified by silica gel column chromatography Yellow solid 5b, yield 51%, purity 96%.

Statistics shows that Sodium 1,2,4-triazol-1-ide is playing an increasingly important role. we look forward to future research findings about 41253-21-8.

Reference:
Patent; Gansu Haotian Chemical Technology Co., Ltd.; Wei Pengfei; Wang Ning; Feng Weiwei; Wang Shixiang; Zhu Yingpu; (8 pag.)CN106397417; (2017); A;,
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. name: Sodium 1,2,4-triazol-1-ide

Production Example 3Synthesis of 5-(4-chlorobenzyl)-2-meth- oxymethoxymethyl-2-methyl- 1 -(1H- 1 ,2,4-triazole- 1-ylmethyl)cyclopentanol (Compound (4)): 10182] 1H-i,2,4-triazolesodium salt (13.1 mmol) was dissolved in NMP (7 ml), and then heated to an internal temperature of 115 C. To this, Compound (6) (8.76 mmol) was added, and the mixture was thoroughly washed with NMP (1.8 ml). After the internal temperature was returned to 115 C., sodium t-butoxide (5.26 mmol) and trimethyl sulfoxonium bromide (1.476 mmol) were gradually added to the mixture over a period of 3 hours. After the addition, the resulting mixture was stirred at a temperature of 115 C. for 75 minutes. After the reaction solution was cooled down to35 C., water was added to the reaction solution, and then extraction with ethyl acetate was performed. An organic layer of the extract was washed with water and saturated brine, and then dried with anhydrous sodium sulfate. The solvent was distilled off, followed by purification of the residue by silica gel column chromatography, and thus Compound (4), which was a mixture of isomers, was obtained.10183] Yield: 71%

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; KUREHA CORPORATION; Miyake, Taiji; Araki, Nobuyuki; Yamazaki, Toru; US2014/94362; (2014); 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. Quality Control of Sodium 1,2,4-triazol-1-ide

EXAMPLE 3; Preparation of crude Anustrozole:Tupsilon the title compound of example 2 (50g) in dry DMF (250ml), anhydrous potassium carbonate (26g) and triazole sodium salt (232 g) are added and the mixture stirred at room 25 temperature for 45 min. Worked up the reaction mixture by adding water ( 1500 ml) and extraction with toluene (3 x 300ml). Combined toluene layer is washed with water (1 x300ml), washed toluene layer is dried over anhydous sodium sulphate, fitered and evaporated toluene to obtain crude anastrozole (4Og) having isomeric impurity 0.5%. EXAMPLE 4Preparation of crude Anastrozole:To the title compound of example 2 (500g) in dry DMF (250ml), anhydrous potassium carbonate (26Og) and triazole sodium salt (2320 g) are added and the mixture stirred at room iemperature for 45 min. Worked up the reaction mixture by adding water ( 15000 ml) and extraction with toluene (3 x 3000ml). Combined toluene layer is washed with water ( 1 3000ml), washed toluene layer is dried over anhydrous sodium sulphate, filtered and evaporated toluene to obtain crude anastrozole (45Og) having isomeric impurity 0.5%. EXAMPLE 5 Preparation of crude Anastrozole:To the title compound of example 2 (5Og) in dry DMF (250ml) anhydrous potassium carbonate (26g) and triazole sodium salt (232 g) are added and the mixture stirred at room temperature for 45 min. Worked up the reaction mixture by adding water (750 ml) and extracting with toluene (3 x 300ml). Combined toluene layer is washed with water ( 1 x300ml).The washed toluene layer is dried over anhydrous sodium sulphate, filtered and evaporated toluene to obtain crude anastrozole (42g) having isomeric impurity 4.52%.EXAMPLE 6Preparation of crude Anastrozole: To the title compound of example 2 (5Og) in dry DMF (250ml) anhydrous potassium carbonate (26g) and triazole sodium salt (232 g) are added and the mixture stirred at room temperature for 45 min. Worked up the reaction mixture by adding water (950 ml) and extracting with toluene (3 x 300ml). Combined toluene layer is washed with water ( 1 x30ml).The washed toluene layer is dried over anhydrous sodium sulphate, filtered and evaporated toluene to obtaincrude anastrozole (42g) having isomeric impurity 2.6%.EXAMPLE7Preparation of crude Anastrozole:To the title compound of example 2 (5Og) in dry DMF (250ml) anhydrous potassium carbonate (26g) and triazole sodium salt (232 g) are added and the mixture stirred at room temperature for 45 min. Worked up the reaction mixture by adding water (2500 ml) and extracting with toluene (3 x 300ml). Combined toluene layer is washed with water ( 1 .300ml).The washed toluene layer is dried over anhydrous sodium sulphate, filtered and evaporated toluene to obtain crude anastrozole (42g) having isomeric impurity 3.2%.

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; SHILPA MEDICARE LTD.; WO2007/105231; (2007); 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

To a solution of (-)(5R-cis)-5-(2,4-difluorophenyl)-5- (iodomethyl)tetrahydiO-3-furanmethanol (7Og) in lambdazetaiV-dimethylformamide (700 ml), 1,2,4- sodium triazole (9Og) and l,3-dimethyl-3,4,5,6-tetrahydro-2(lH)-pyrimidinone (17.7 ml) were added at ambient temperature. The resulting mixture was heated to 100 C and stirred for 24 hours. After completion of reaction (monitored by TLC),the reaction mass was cooled and quenched with demineralized water. The product was extracted with dichloromethane (2x500ml). The organic layer was treated with 6N hydrochloric acid (400 ml). The layers were separated and pH of the aqueous layer is adjusted to 8-9 with aqueous sodium hydroxide (50% w/v). The product from aqueous layer was extracted with ethyl acetate (2x500ml) and subsequently organic layer was washed with brine and dried over sodium sulfate. The solvent was removed to obtain 42g of the title compound.

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; IND-SWIFT LABORATORIES LIMITED; WO2009/141837; (2009); A2;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Related Products of 41253-21-8, 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.

[Step 1] Synthesis of ethyl 2-methyl-2-(1H-1,2,4-triazol-1-yl)propanoate: At room temperature, cesium carbonate (5.0 g, 15 mmol) and sodium 1,2,4-triazol-1-ide (0.58 g, 6.2 mmol) were added to a solution of ethyl 2-bromo-2-methylpropanoate (1.0 g, 5.1 mmol) in DMF (25 mL). The resulting reaction solution was stirred at 50C for 24 hours, and then concentrated under reduced pressure. Water was added to the obtained crude product, and extraction with chloroform was carried out. The organic layer was dried over anhydrous sodium sulfate, and then concentrated under reduced pressure, followed by purifying the obtained crude product by silica gel column chromatography (eluent, hexane:ethyl acetate = 7:3 ? 4:6), to obtain 0.84 g (89%) of ethyl 2-methyl-2-(1H-1,2,4-triazol-1-yl)propanoate (hereinafter referred to as Reference Example Compound 40).

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; Toray Industries, Inc.; NISHIMURA, Yutaka; KATO, Yuko; HAYASHI, Shinnosuke; YAMAZAKI, Aiko; YAMAMOTO, Masashi; ASAOKA, Yoshiji; YAMADA, Masateru; YAMADA, Naohiro; EP2832724; (2015); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Application of 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.

To a solution of 2,4-difluorobenzonitrile (10 g, 72 mmol) dissolved in tetrahydrofuran (20 mL), and dimethylformamide (40 mL) was added 1,2,4-triazole sodium salt (6.3 g, 70 mmol) and the mixture stirred at 90 C. for 3 h after which the mixture was filtered and the solvent removed. The resulting residue was adsorbed onto silica gel and intermediates 67 and 68 separated by flash chromatography, eluting with 0% to 30% ethyl acetate/hexanes. Colorless needles (2.46 g, 18% yield) 1H NMR (500 MHz, CDCl3) ?: 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.To a solution of 2,4-difluorobenzonitrile (10 g, 72 mmol) dissolved in tetrahydrofuran (20 mL), and dimethylformamide (40 mL) was added 1,2,4-triazole sodium salt (6.3 g, 70 mmol) and the mixture stirred at 90 C. for 3 h after which the mixture was filtered and the solvent removed. The resulting residue was adsorbed onto silica gel and intermediates 67 and 68 separated by flash chromatography, eluting with 0% to 30% ethyl acetate/hexanes. White solid (0.746 g, 6% yield) 1H NMR (500 MHz, CDCl3) ?: 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.

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

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

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.

1-2. Preparation of 1-(3-chloropropyl)-1,2,4-triazole (compound of formula 3) A 1,2,4-triazole sodium salt (5g, 54.91mmol) was dissolved in dimethylformamide (50mL) and the solution was cooled to 0. Then, sodium hydride (60%, 2.86g, 71.38mmol) was added thereto, followed by stirring for 30 minutes. 1-bromo-3-chloropropane (6.5mL, 65.89mmol) was added thereto, followed by stirring at room temperature for 12 hours, and the reaction was terminated with the addition of an ammonium chloride saturated solution. After extraction with ethyl acetate and water, the organic layer was washed with brine, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The resulting residue was purified by column chromatography to afford the title compound (2.77g, 35%).1H NMR (CDCl3, 400MHz): delta 8.08 (s, 1H), 7.94 (s, 1H), 4.36 (t, J =6.4Hz, 2H), 3.45 (t, J =6Hz, 2H), 2.35-2.30 (m, 2H).

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; DONG-A PHARM.CO., LTD.; KIM, Soon-Hoe; IM, Weon-Bin; CHOI, Sung-Hak; CHOI, Sun-Ho; SOHN, Ju-Hee; SUNG, Hyun-Jung; KIM, Mi-Yeon; CHO, Kang-Hun; SOHN, Tae-Kyoung; WO2011/132901; (2011); A2;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics