Tag: M.W=0-100

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. 288-36-8, name is 1H-1,2,3-Triazole, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: C2H3N3

Method B: 2-Fluoro-6-[1 ,2,3]triazol-2-yl-benzoic acid. To a 2 L, 3- necked, round-bottomed flask equipped with an overhead mechanical stirrer, thermocouple probe, heating mantle, reflux condenser, and nitrogen inlet were added 2-fluoro-6-iodobenzoic acid (127.6 g, 480 mmol), copper iodide (4.57 g, 24 mmol), and Cs2C03 (312.6 g, 959 mmol). To these solids were added dioxane (640 mL), then water (2.6 mL, 144 mmol), then 1 H-1 ,2,3-triazole (55.6 mL, 959 mmol), and finally frans-1 ,2-dimethylcyclohexane-1 ,2-diamine (15.1 mL, 96 mmol). The mixture was then warmed to 60 C for 30 min, then to 83 C for 30 min, and then to 100 C for 3 h. After the 3 h at 100 C, the mixture was cooled and then 1 L of MTBE and 1 L of water were added. After vigorous mixing, the layers were separated and the bottom aqueous layer was acidified to pH 1 .72 with -148 mL of concentrated hydrochloric acid. The aqueous was then extracted twice with EtOAc. The combined organic layers were dried over Na2S04, filtered, and concentrated to provide a dark oil. The oil was stirred overnight in EtOAc (450 mL) and the resulting precipitate was removed by filtration. The mother-liquors were concentrated to a brown solid (106.21 g, 75 wt% by quantitative HPLC, 79.7 g, 80%). 1H NMR (400 MHz, DMSO-d6): 8.22 – 8.13 (bs, 2H), 7.84-7.80 (m, 1 H), 7.74 – 7.65 (m, 1 H), 7.50 – 7.41 (m, 1 H).

According to the analysis of related databases, 288-36-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; JANSSEN PHARMACEUTICA NV; LETAVIC, Michael; RUDOLPH, Dale, A.; SAVALL, Brad, M.; SHIREMAN, Brock, T.; SWANSON, Devin; WO2012/145581; (2012); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 584-13-4, name is 4H-1,2,4-Triazol-4-amine, 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 584-13-4, Quality Control of 4H-1,2,4-Triazol-4-amine

General procedure: 4-Carboxybenzenesulphonamide (10.0mmol), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (EDCI, 12.0mmol), and 1-hydroxybenzotriazole (HOBt, 12.0mmol) were added to 10mLN,N-dimethylformamide (DMF) and stirred at room temperature (20-25C) for 30min. Then, 2-amino-4-ethoxycarbonyl thiazole (12.0mmol) and 4-dimethylaminopyridine (DMAP, 3.0mmol) were added to the solution. The reaction was carried out at 45C for 24h. The mixture was cooled to room temperature and extracted with ethyl acetate (EtOAc). The combined organic layers were washed with brine, dried over anhydrous Na2SO4, filtered, and concentrated under reduced pressure. The crude product was purified by column chromatography (dichloromethane/methanol, 60:1-30:1) to recover compound 2a. The method for synthesising 2b-3f was the same as for 2a.

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, 4H-1,2,4-Triazol-4-amine, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Cheng, Yunyun; Feng, Yan; He, Xinhua; Li, Zhenwang; Sun, Xianyu; Wang, Jing; Yang, Chaofu; Yang, Xu; Zhang, Jiwen; Zhao, Wangyu; Zhuang, Xiaomei; Bioorganic Chemistry; vol. 100; (2020);,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Reference of 7170-01-6, 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. 7170-01-6, name is 3-Methyl-1H-1,2,4-triazole belongs to triazoles compound, it is a common compound, a new synthetic route is introduced below.

EXAMPLE 8 In a sealed tube dicarbonyl intermediate 10 (50 mg, 0.13 mmol), 3-methyl-1,2,4-triazole (52 mg, 0.75 mmol) and copper powder (16 mg, 0.25 mmol) were combined and heated at 140 C. with microwaves for 1 h. The reaction was diluted with MeOH (3 mL), filtered through celite and the filtrate was purified by preparative HPLC to yield 16 (3 mg, 0.007 mmol, 5%) as a yellow solid. 1H NMR: (500 MHz, CD3OD) delta 8.97 (s, 1H), 8.61 (s, 1H), 8.28 (s, 1H), 8.27 (s, 1H), 7.52-7.40 (m, 5H), 4.02-3.44 (m, 8H); LC/MS: (ES+) m/z (M+H)+=431; HPLC Rt=0.82 min., column G, conditions B.

The synthetic route of 3-Methyl-1H-1,2,4-triazole has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Bender, John A.; Yang, Zhong; Kadow, John F.; Meanwell, Nicholas A.; US2005/124623; (2005); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Application of 7170-01-6, 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. 7170-01-6, name is 3-Methyl-1H-1,2,4-triazole belongs to triazoles compound, it is a common compound, a new synthetic route is introduced below.

((2S,3S)-3-(((benzyloxy)carbonyl)amino)-1-(2,4-dimethoxybenzyl)-4-oxoazetidin-2-yl)methyl methanesulfonate (3.74 g, 8.0 mmol), 3-methyl-1H-1,2,4-triazole (2.00 g, 24.0 mmol), K2CO3 (6.64 g, 48.0 mmol) and NaI (2.88 g, 17.2 mmol) were slurried in DMF (16 mL) and heated to 70 C. with stirring. After 24 h the mixture was concentrated in vacuo. The crude residue was purified via silica gel chromatography (MeOH-DCM, 2%) to afford title compounds (1.64 g, 44% combined) as an off-white solid (unseperable mixture). LCMS: m/z=466.2 (M+1).

The synthetic route of 3-Methyl-1H-1,2,4-triazole has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NOVARTIS AG; AULAKH, Virender Singh; CASAREZ, Anthony; LIN, Xiaodong; LINDVALL, Mika; MCENROE, Glenn; MOSER, Heinz Ernst; RECK, Folkert; TJANDRA, Meiliana; SIMMONS, Robert Lowell; YIFRU, Aregahegn; ZHU, Qingming; US2015/266867; (2015); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Related Products of 1455-77-2, A common heterocyclic compound, 1455-77-2, name is 3,5-Diamino-1,2,4-triazole, molecular formula is C2H5N5, 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.

Included at room temperature3,5-diamino-1,2,4-triazole 15.0 g (0.151 mol)And dehydrated N,N-dimethylformamide 100mLAdd 28percent to the suspensionSodium methoxide methanol solution 29.2g (0.151mol)After making a uniform solution and stirring for 30 minutes,30.1 g (0.151 mol) of 3-chloropropyltrimethoxydecane was added.Stir at 77~80 ¡ã C for 4 hours.After cooling the suspension reaction solution to 3 ¡ã C,Filter out insoluble matter,And the solvent of the filtrate is distilled off under reduced pressure,Obtained 35.7 g (0.137 mol, brown viscous,Yield 90.5percent).

The synthetic route of 1455-77-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SHIKOKU CHEMICALS CORPORATION; MURAI,, TAKAYUKI; TANIOKA, MIYA; IIDA, SHUSAKU; KATSUMURA, MASATO; YAMAJI, NORIAKI; IMAMINE, TAKAHITO; TSUJINO, MASAHIKO; HIRAO, HIROHIKO; (52 pag.)TW2018/41929; (2018); A;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 288-88-0, name is 1H-1,2,4-Triazole, 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 288-88-0, Safety of 1H-1,2,4-Triazole

To a solution (3 ML) of 1,2,4-triazole (0.259 g, 3.75 mmol) in N,N-dimethylformamide was added small portions of sodium hydride (60% dispersion in oil, 0.12 g, 3.0 mmol) at about 20 C., and the mixture was stirred for about 3 hr until hydrogen was not generated.To a solution of sodium salt of 1,2,4-triazole thus obtained was added dropwise a solution (5.5 ML) of the total amount of (2R,3R)-3-(2′,4′-difluorophenyl)-3,4-epoxy-2-methanesulfonyoxybutane obtained above in N,N-dimethylformamide at room temperature.The mixture was stirred at 75-80 C. for 1.5 hr.The reaction mixture was added dropwise to water (20 ML), and the mixture was extracted 3 times with ethyl acetate (20 ML).The extracted ethyl acetate layers were mixed, and the mixture was washed twice with saturated brine (10 ML) and dried over anhydrous magnesium sulfate.After filtration, the filtrate (ethyl acetate solution) was concentrated and the obtained concentrate was subjected to silica gel column chromatography (SiO2, 5 g) and eluted with n-heptane-ethyl acetate (10:1)ethyl acetate.The objective fraction was concentrated to give a pale-yellow oil (0.297 g).The obtained pale-yellow oil was crystallized from a mixed solvent of ethyl acetate (1 ML)-n-heptane (4 ML) to give the title compound (0.185 g, yield from (2R)-2′,4′-difluoro-2-hydroxypropiophenone: 44%).As a result of analysis by HPLC, the optical purity was 100% e.e.

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; Sumika Fine Chemicals Co., Ltd.; US2003/236419; (2003); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 16681-65-5, name is 1-Methyl-1H-1,2,3-triazole, 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 16681-65-5, Safety of 1-Methyl-1H-1,2,3-triazole

Intermediate 18: 1-Methyl-1H-1,2,3-triazole-5-carbaldehydeThe title compound was prepared according to the patent application WO2008/135826. To a 50 mL 2-necked flask containing 1-methyl-1H-1,2,3-triazole (1.0 g, 12.0 mmol, prepared according to PCT Int. AppL 2008098104) was added THF (45 mL) and the colorless solution was cooled to -40 C. Then, n-BuLi (2.5 M in hexanes, 4.8 mL, 12.0 mmol) was added dropwise which afforded a dark reddish-brown viscous solution. The mixture was stirred between -30 to -20 C for 45 minutes, then neat DMF (3 mL, 38,5 mmol) was introduced at -10 C. The mixture was allowed to warm up to room temperature and stirred for 60 minutes, followed by pouring into water. The aqueous portion was extracted with EtOAc (4 x 50 mL) and the combined organics were washed with brine, dried over MgSO4, filtered and concentrated. The aqueous portion was back- extracted with DCM (3 x 50 mL) and dried as above. The combined organics were concentrated to give a light brown oil that was much more UV active than the starting material, TLC in either 25% CH3CN-DCM or 25% EtOAc-DCM showed the product to have a slightly higher Rf than the starting material. Chromatography on silica gel (100% DCM increasing to 25% CH3CN-DCM) provided the title compound as a colorless oil.

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; JANSSEN PHARMACEUTICA NV; LEONARD, Kristi, A.; BARBAY, Kent; EDWARDS, James, P.; KREUTTER, Kevin, D.; KUMMER, David, A.; MAHAROOF, Umar; NISHIMURA, Rachel; URBANSKI, Maud; VENKATESAN, Hariharan; WANG, Aihua; WOLIN, Ronald, L.; WOODS, Craig, R.; FOURIE, Anne; XUE, Xiaohua; CUMMINGS, Maxwell, D.; WO2015/57206; (2015); 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. 7170-01-6, name is 3-Methyl-1H-1,2,4-triazole, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 3-Methyl-1H-1,2,4-triazole

A mixture of tris(dibenzylideneacetone)dipalladium(0) (98%, 94.7 mg, 0.101 mmol) and di-tert-butyl[3,4,5,6-tetramethyl-2?,4?,6?-tri(propan-2-yl)biphenyl-2-yl]phosphane (95%, 103 mg, 0.203 mmol) in toluene (10 mL) was degassed with nitrogen for 5 minutes, then heated at 125 C. for 3 minutes. In a separate flask, a mixture of C43 (1.70 g, 3.38 mmol), 3-methyl-1H-1,2,4-triazole (561 mg, 6.75 mmol), and potassium phosphate (1.48 g, 6.97 mmol) in toluene (10 mL) and 1,4-dioxane (10 mL) was degassed with nitrogen for 10 minutes. The catalyst solution was transferred to the reaction flask via syringe, and the reaction mixture was heated at 125 C. for 2 hours, whereupon it was partitioned between water and ethyl acetate. The organic layer was dried over sodium sulfate, filtered, and concentrated in vacuo; silica gel chromatography (Gradient: 50% to 100% ethyl acetate in heptane) provided the product as an off-white solid. Yield: 1.3 g, 2.6 mmol, 77%. LCMS m/z 506.4 [M+H]+. 1H NMR (400 MHz, CDCl3), characteristic peaks: delta 9.52 (br s, 1H), 8.21 (d, J=7.9 Hz, 1H), 7.38 (d, J=7.8 Hz, 1H), 7.25-7.31 (m, 1H, assumed; partially obscured by solvent peak), 6.68 (d, J=10.0 Hz, 1H), 5.05 (d, J=15.2 Hz, 1H), 4.20-4.32 (m, 2H), 3.53-3.62 (m, 1H), 3.14 (d, J=15.2 Hz, 1H), 2.49 (s, 3H), 1.84 (s, 3H), 1.00 (d, J=6.6 Hz, 1H), 0.69 (d, J=6.5 Hz, 1H).

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 7170-01-6.

Reference:
Patent; Pfizer Inc.; Pettersson, Martin Youngjin; am Ende, Christopher William; Johnson, Douglas Scott; Kauffman, Gregory Wayne; Stepan, Antonia Friederike; Verhoest, Patrick Robert; (64 pag.)US2016/222007; (2016); 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

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 16681-65-5 as follows. Quality Control of 1-Methyl-1H-1,2,3-triazole

To a flask containing 1-methyl-1H-1,2,3-triazole (111 mg, 1.34 mmol) was added THF (10 mL) and the solution was cooled to -45 C. using a CH3CN-CO2 bath. n-BuLi (2.5 M in hexanes, 0.5 mL, 1.25 mmol) was added dropwise to provide a white suspension. The suspension was stirred at -45 C. for 25 minutes. A pre-warmed THF solution of (2,4-dichloro-3-(2,2,2-trifluoroethyl)quinolin-6-yl)(1,2-dimethyl-1H-imidazol-5-yl)methanone (470 mg, 1.17 mmol in 7 mL THF, Intermediate 70) was introduced at -45 C. The reaction temperature was allowed to warm gradually to room temperature over 70 minutes then quenched with aqueous NH4Cl solution. The aqueous portion was extracted with EtOAc (3*40 mL), and the combined organics were washed with brine, dried over MgSO4, filtered and concentrated. Chromatography on silica gel (2% MeOH-DCM increasing to 8% MeOH) afforded the title compound as a tan amorphous solid. MS (ESI): mass calcd. for C20H17Cl2F3N6O, 484.1. found, 485.0 (M+H)+. 1H NMR (500 MHz, CDCl3) delta ppm 8.60 (s, 1H), 8.44-8.40 (m, 2H), 7.95 (d, J=8.8 Hz, 1H), 7.62 (dd, J=8.8, 1.8 Hz, 2H), 6.95 (s, 1H), 5.89 (s, 1H), 4.05 (q, J=9.6 Hz, 2H), 3.89 (s, 3H), 3.32 (s, 3H).

According to the analysis of related databases, 16681-65-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; JOHNSON & JOHNSON; LEONARD, KRISTI A.; BARBAY, KENT; EDWARDS, JAMES P.; KREUTTER, KEVIN D.; KUMMER, DAVID A.; MAHAROOF, UMAR; NISHIMURA, RACHEL; URBANSKI, MAUD; VENKATESAN, HARIHARAN; WANG, AIHUA; WOLIN, RONALD L.; WOODS, CRAIG R.; FOURIE, ANNE; XUE, XIAOHUA; CUMMINGS, MAXWELL D.; MCCLURE, KELLY; TANIS, VIRGINIA; US2015/111870; (2015); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics