Day: January 25, 2021

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 3641-13-2 as follows. Quality Control of 5-Amino-4H-1,2,4-triazole-3-carboxylic acid

0.2mmol, 0.0252g H2atrc, 0.2mmol, 0.0389g 4,4?-bipy and 0.2mmol, 0.0520g CdSO4¡¤8/3H2O mixed with 10mL H2O and 5mL EtOH were placed in a 25mL Teflon-lined stainless-steel autoclave. The mixture was kept inside a furnace at 110C for 5 days, and then naturally cooled to ambient temperature. The colorless platelet crystals of 1 suitable for X-ray diffraction were collected after soak clearing with water and ethanol. Yield based on Hatrz: 23.1mg, 39.48%. IR data (in KBr, cm-1) for 1: 3428(m), 3339(m), 3268(w), 3204(w), 3147(w), 2987(w), 2859(w), 1643(m), 1592(m), 1528(w), 1413(w), 1362(w), 1278(w), 1125(s), 1055(m), 882(w), 805(w), 600(w), 460(w).

According to the analysis of related databases, 3641-13-2, the application of this compound in the production field has become more and more popular.

Reference:
Article; Liu, Bing; Feng, Hui-Jun; Zhang, Zong-Hui; Xu, Ling; Jiao, Huan; Journal of Molecular Structure; vol. 1098; (2015); p. 240 – 245;,
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. 15988-11-1, name is 4-Phenyl-1,2,4-triazolidine-3,5-dione, A new synthetic method of this compound is introduced below., Computed Properties of C8H7N3O2

General procedure: A mixture of dimedone (1, 1 mmol), 4-phenylurazole (2, 1 mmol), aromatic aldehyde (3a-h, 1mmol) and S-LCCO nano perovskite (0.01 g) was mixed in a high-pressure Teflon reactor, which was equipped with a magnetic stirrer and an optical fiber, which was implemented to control the reaction’s temperature. The reaction mixture was irradiated by 400 W microwave at 80 oC, for the specified reaction times. TLC with n-hexan:ethylacetate eluent was used to monitor the progress of the reactions. After reaction completion and cooling, the reaction mixtures were filtered and washed with ethanol to separate the catalyst. First, 10 mL water was added to the solution. Then, EtOH/H2O (4:1) was added to crystallize the water insoluble crude products. Then the crystals were filtered to achieve pure products (4a-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:
Article; Zahedi, Najmeh; Javid, Ali; Mohammadi, Mohammad Kazem; Tavakkoli, Haman; Bulletin of the Chemical Society of Ethiopia; vol. 32; 2; (2018); p. 239 – 248;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Some common heterocyclic compound, 15294-81-2, name is 4,5-Dibromo-1H-1,2,3-triazole, molecular formula is C2HBr2N3, 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. Quality Control of 4,5-Dibromo-1H-1,2,3-triazole

Example 160: Preparation of 4,5-dibromo-l-methyl-lH-[1.2.31triazole and 4,5-dibromo- 2-methyl-2H-r 1 ,231triazole(A) (B)To a solution of 4,5-dibromo- IH-[1, 2,3]triazole (2.26 g, 10 mmol) (Example 159) and triethyl amine (1.5 ml, 10 mmol) in dichloromethane (50 ml), was added methyl iodide (625 mul, 10 mmol). The reaction mixture was stirred at room temperature for 24 hours. More triethyl amine (0.75 ml, 5 mmol) and more methyl iodide (312 mul, 5 mmol) were added and the mixture was stirred for 3 hours. The reaction mixture was quenched with aqueous ammonium chloride (saturated, 15 ml). The organic extract was dried over magnesium sulfate and concentrated and the residue was purified by column chromatography on silica gel (eluent 10-30% ethyl acetate in hexane) to give 4,5-dibromo-2- methyl-2H-[l ,2,3]triazole (isomer B) (625 mg, 26% yield) and 4,5-dibromo- 1-methyl- IH-[1, 2,3]triazole (isomer A) (825 mg, 34% yield). Isomer A 1H-NMR (400 MHz, CDCl3): 4.09 (s, 3H, Me) ppm. Isomer B 1H-NMR (400 MHz, CDCl3): 4.18 (s, 3H, Me) ppm.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 15294-81-2, its application will become more common.

Reference:
Patent; SYNGENTA LIMITED; WO2007/71900; (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. 16681-70-2, name is 1H-[1,2,3]Triazole-4-carboxylic acid belongs to Triazoles compound, it is a common compound, a new synthetic route is introduced below. Product Details of 16681-70-2

[0758] 3H-1,2,3-triazole-5-carboxylic acid (2.5 mg, 22f.tmol) was combined with HATU (8.4 mg, 22 flillOl) in DMF(0.3 mL) and stirred for 10 minutes; Et3N (1 eq.) was addedand the mixture was stirred for 1 minute. Compound 2 (22f.tmol) was dissolved in DMF (0.5 mL) and Et3N (3.1 f.LL, 22f.tmol) was added, followed by addition of the activated acidsolution. The mixture was stirred for 30 minutes and concentratedto yieldCompound3, which was carried to the next stepwithout purification.

The synthetic route of 16681-70-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; THERAVANCE BIOPHARMA R&D IP, LLC; Fleury, Melissa; Beausoliel, Anne-Marie; Hughes, Adam D.; Long, Daniel D.; Wilton, Donna A.A.; US2015/210690; (2015); 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. 10570-40-8, name is 4-Methyl-4H-1,2,4-triazole, A new synthetic method of this compound is introduced below., category: Triazoles

4.2 1-(4-Methyl-4H-1,2,4-triazol-3-yl)octan-1-ol To a solution of 4-methyl-1,2,4-triazole (681 mg, 7.78 mmol), TMEDA (0.40 ml) in dry THF (10 ml) and at -60 C, 2.69 M n-BuLi solution (2.9 ml, 7.80 mmol) was added drop wise. After stirring at -60 C for 30 min, 10 ml of dry THF solution of octanol (1.30 mL, 8.33 mmol) was added and the mixture was stirred for additional 4 h at -60 C to -30 C. Then H2O was added and the mixture was extracted three times with ethyl acetate. The organic layer was washed with saturated brine and dried over Na2SO4 and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (1-5% methanol/chloroform) as a colorless solid (1.13 g, 69%): Mp. 63-65 C; 1H NMR (500 MHz, CDCl3) delta 0.87 (3H, t, J = 6.6 Hz), 1.30-1.26 (9H, m), 1.46 (1H, q, J = 5.2 Hz), 1.93-1.84 (2H, m), 3.50 (1H, br s), 3.93 (3H, s), 4.82 (1H, q, J = 6.3 Hz), 7.76 (1H, s); 1H NMR (300 MHz, DMSO) delta 0.88 (3H, t, J = 6.9 Hz), 1.26-1.49 (14H, m), 1.87-1.93 (2H, m), 2.70 (1H, d, J = 7.5 Hz) 3.92 (3H, s), 4.84 (1H, q, J = 6.9 Hz), 7.79 (1H, s); 13C NMR (126 MHz) delta 14.1, 22.7, 25.2, 29.5, 31.9, 33.7, 35.4, 39.8, 64,2, 143.6, 155.0; HRMS (ESI) m/z calcd for C11H21N3NaO (M + Na)+ 234.1582, found. 234.1573.

The synthetic route of 10570-40-8 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Suzuki, Yumiko; Iwata, Naoto; Dobashi, Kohei; Takashima, Ryo; Arulmozhiraja, Sundaram; Ishitsubo, Erika; Matsuo, Naoya; Tokiwa, Hiroaki; Tetrahedron; vol. 74; 3; (2018); p. 392 – 400;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Related Products of 135242-93-2,Some common heterocyclic compound, 135242-93-2, name is (1-Methyl-1H-[1,2,4]triazol-3-yl)methanol, molecular formula is C4H7N3O, 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 a solution of 0.5 g (4.42 mmol, 1.0 eq.) of (l-methyl-li/-l,2,4-triazol-3-yl)methanol (Xlla) in 20 mL of acetonitrile was added 1.07 g (6.63 mmol, 1.5 eq.) of I,G -carbonyl and the mixture was stirred at room temperature for 2 h. Volatiles were removed in vacuo and the residue was resuspend in 20 mL of water. The mixture was extracted with 3 x 50 mL of 5% methanol in methylene chloride. The combined organic extracts were washed with 50 mL of sat. sodium carbonate solution, followed by 50 mL of brine, dried (T^SCL), filtered and the solvent was removed in vacuo to provide 0.77 g of ( 1 -methyl- 1 H- 1 2.4-triazol-3-yl)methyl 1 //-imidazole- 1 -carboxy late (XIHa).

The synthetic route of 135242-93-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ARBUTUS BIOPHARMA CORPORATION; KULTGEN, Steven; COLE, Andrew G.; (217 pag.)WO2020/23710; (2020); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Some common heterocyclic compound, 7343-33-1, name is 5-Bromo-1H-1,2,4-triazole, molecular formula is C2H2BrN3, 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. SDS of cas: 7343-33-1

Step 1: 3-Bromo-1-(4-methoxybenzyl)-1H-1,2,4-triazole A mixture of 3-bromo-1H-1,2,4-triazole (10.0 g, 67.6 mmol), 1-(chloromethyl)-4-methoxybenzene (10.6 g, 67.6 mmol), DIPEA (17.5 g, 135 mmol) and potassium iodide (5.61 g, 33.8 mmol) in acetonitrile (300 mL) was stirred at 65¡ã C. for 120 min. The solvent was evaporated in vacuo and the residue was purified via flash chromatography on silica gel (solvent gradient: 0-30percent ethyl acetate in petroleum ether) to yield 12.9 g (71percent) of the title compound as a white solid. LCMS (ESI): [M+H]+=268/270.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 7343-33-1, its application will become more common.

Reference:
Patent; Genentech, Inc.; Braun, Marie-Gabrielle; Garland, Keira; Hanan, Emily; Purkey, Hans; Staben, Steven T.; Heald, Robert Andrew; Knight, Jamie; Macleod, Calum; Lu, Aijun; Wu, Guosheng; Yeap, Siew Kuen; (183 pag.)US2018/65983; (2018); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Synthetic Route of 16681-70-2, 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. 16681-70-2, name is 1H-[1,2,3]Triazole-4-carboxylic acid belongs to Triazoles compound, it is a common compound, a new synthetic route is introduced below.

Preparation of N’-t-butyl-N-(1,2,3-triazole-4-carbonyl)-N’-(3-methylbenzoyl)hydrazine 1,2,3-triazole-4-carboxylic acid (1.0 g) and triethylamine (0.9 g) were dissolved in 40 ml methylene chloride and cooled in an ice bath. Methanesulfonylchloride (1.0 g) was added dropwise. After addition was complete, the reaction mixture was stirred for 0.5 hours. N’-t-butyl-N’-(3-methylbenzoyl)hydrazine (1.84 g) in 10 ml CH2 Cl2 was added dropwise. The resulting mixture was allowed to stand for 14 hours. Aqueous sodium bicarbonate was added. The organic layer was dried over anhydrous magnesium sulfate, filtered and evaporated to give a yellow oil. Chromatography on silica gel using acetone as eluant afforded N’-t-butyl-N-1,2,3-triazole-4-carbonyl-N’-(3-methylbenzoyl)hydrazine.

The synthetic route of 1H-[1,2,3]Triazole-4-carboxylic acid has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Rohm and Haas Company; US6013836; (2000); A;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Synthetic Route of 74205-82-6, These common heterocyclic compound, 74205-82-6, name is (1H-1,2,4-Triazol-1-yl)methanol, 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.

Example4. Synthesis of Intermediate 5Intermediate 4 (16.3g, 70.4 mmol) was completely dissolved in concentrated sulfuric acid (80ml) under ice bath, and triazolemethanol (10.4g) was added. The solution was stirred at room temperature for 5hrs. TLC was used toshow the completion of raw materials. Post-treatment: the reaction solution wasslowly added to 20% sodium hydroxide solution under ice bath. After alkalizing,dichloromethane was added to extract the product. The organic layer was driedand the solvent was removed by rotary evaporation. 21.2g yellow oil product(crude) was obtained. 15.6g light yellowsemi-solid (Intermediate 5) was obtained after column chromatography separation(dichloromethane: methanol 20: 1+ 1% triethylamine) and rotary evaporation,with a yield of 71.0%.

The synthetic route of 74205-82-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Sichuan University; Wu, Yong; Hai, Li; Sun, Baohou; He, Yi; Li, Xiaocen; (11 pag.)CN103664900; (2016); B;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Application of 103755-58-4, 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. 103755-58-4 name is (1-Phenyl-1H-1,2,3-triazol-4-yl)methanol, 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.

General procedure: Into a round bottom flask was added 5.71mmolof triazole type 12 or 21a in 50mL of dry THF, 17.13mmolof sodium hydride and 57.1mmolof alkyl bromide. The mixture was heated to reflux, and reaction progress was monitored by TLC. Subsequently, the solvent was evaporated and the mixture was extracted with ethyl acetate, washed with distilled water (3¡Á100mL) and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the product was purified via silica-gel column chromatography using a gradient mixture of hexane-ethyl acetate, to afford the pure derivatives 14a-g and 23a-b.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, (1-Phenyl-1H-1,2,3-triazol-4-yl)methanol, and friends who are interested can also refer to it.

Reference:
Article; Gonzaga, Daniel; Senger, Mario Roberto; Da Silva, Fernando De Carvalho; Ferreira, Vitor Francisco; Silva Jr., Floriano Paes; European Journal of Medicinal Chemistry; vol. 74; (2014); p. 461 – 476;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics