Day: July 14, 2021

Research speed reading in 2021. Redox catalysis has been broadly utilized in electrochemical synthesis due to its kinetic advantages over direct electrolysis. 60166-43-0, name is 1,4-Dimethyl-1H-1,2,3-triazole belongs to triazoles compound, it is a common compound, a new synthetic route is introduced below. category: Triazoles

A solution of 1,4-dimethyltriazole (14.1, 500 mg, 5.15 mmol, 1 equivalent) in THF (2 mL) was added dropwise to a solution of n-BuLi (2.5 M, 2.47 mL, 1.2 equivalent) in THF (15 mL) at -78 C. under nitrogen atmosphere. The resulting cloudy mixture was stirred at -70 C. for 1 h. After this time, tributyl tinchloride (1.84 g, 5.66 mmol, 1.52 mL, 1.1 equivalent) was added; the reaction mixture became clear and was stirred at -70 C. for 30 min, then it was allowed to warm to 20 C. The reaction mixture was poured into saturated NH4Cl solution (10 mL) and extracted with EtOAc (50 mL*3). The combined organic layers were washed with brine (50 mL*2), were dried over sodium sulfate then filtered. The solvent was concentrated under reduced pressure to give tributyl-(3,5-dimethyltriazol-4-yl)stannane (14.2, 2.2 g) as a yellow oil; LCMS [M+1]: 388.2.

Balanced chemical reaction does not necessarily reveal either the individual elementary reactions by which a reaction occurs or its rate law. In my other articles, you can also check out more blogs about 60166-43-0, and we look forward to future research findings.

Reference:
Patent; Mirati Therapeutics, Inc.; Marx, Matthew Arnold; Lee, Matthew Randolph; Galemmo, Robert Anthony; Bobinski, Thomas P.; US2018/265517; (2018); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Research speed reading in 2021. We’ll be discussing some of the latest developments in chemical about CAS: 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. Recommanded Product: 7170-01-6

The solution of compound 1 (30 g, 0.13 mol) in THF (1.5 L) was cooled to -78 C. Then a solution of vinyl magnesium in THF (508 mL, 1N, 0.51 mol) was added dropwise to the above solution maintained below -40 C. The mixture was stirred for 3 hrs at -78 C before being quenched with saturated aqueous NH4Cl solution. The layers were separated, the aqueous layer was extracted with EtOAc (3×500 mL) and the combined organic layer was washed with brine and concentrated. The crude product was purified by silica gel column chromatography to obtain compound 2 (5 g, 17%). Compound 2 (4.0 g, 17.2 mmol) was dissolved in freshly prepared NaOMe (20 mL). CuI (3.2 g, 17.2 mmol) was added to the above solution. The mixture was stirred at 110 C under microwave for 3 hrs. After the mixture was completed, the mixture was added EtOAc and H2O, then the suspension was filtered, the filtrate was separated. The organic layer was concentrated to give crude product which was purified by column chromatography to give compound 3 (1.8 g, 45%). A mixture of compound 3 (0.7 g, 3.8 mmol) and 3-methyl-1,2,4-triazole (6.4 g, 76.8 mmol) was added copper powder (0.49 g, 7.68 mmol) and KOH (0.43 g, 7.68 mmol). The mixture was heated tomelt at 170-175 C under N2. After the starting material was consumed completely, the mixture was added EtOAc and H2O, then the suspension was filtered, the filtrate was separated. The organic layer was concentrated to give crude product which was purified by column chromatography to give compound 4 (0.23 g, 26%). A solution of compound 4 (0.23 g, 1 mmol) in THF (12 mL) was cooled to -10 C, EtMgBr (0.47 g, 3.5 mmol)was added dropwise at -10 C followed by the addition of pyridine(0.3 mL). The slurry was cooled to -45 C, and the ethyl 2-chloro-2-oxoacetate (0.55 g, 4 mmol) was added dropwise at -45 C. The slurry was allowed to -10 C and stirred at this temperature for 1h. After the reaction was completed, the mixture was quenched with IPA (2mL) and H2O (20 mL). The mixture was extracted with EtOAc, the organic layer was washed with brine and concentrated to give crude product which was purified by column chromatographyto give compound 5 (0.17 g, 52%). A solution of compound 5 (0.17 g, 0.52mmol) in MeOH (5 mL) was added NaOH (0.041 g, 1.03 mmol) and H2O (2mL). The mixture was stirred at 25 C for 6 hrs and then added 1N HCl to adjusted pH 6, the mixture was concentratedto give compound 6 (0.29 g) as crude product.

In conclusion, we affirm that quantitative kinetic descriptions of catalytic behavior continue to serve as an indispensable tool to navigate research efforts intended to model. Read on for other articles about 7170-01-6.

Reference:
Article; Tuyishime, Marina; Lawrence, Rae; Cocklin, Simon; Bioorganic and Medicinal Chemistry Letters; vol. 26; 1; (2016); p. 228 – 234;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Related Products of 956317-36-5, New Advances in Chemical Research in 2021. Chemo-enzymatic cascade processes are invaluable due to their ability to rapidly construct high-value products from available feedstock chemicals in a one-pot relay manner. 956317-36-5, name is 5-Methyl-2-(2H-1,2,3-triazol-2-yl)benzoic acid, molecular formula is C10H9N3O2, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, below Introduce a new synthetic route.

General procedure: 1-(3-Dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride(WSCHCl) (37.4 g, 0.20 mol) was added to a solution of Nethyl-2[3-(5-fluoro-pyridin-2-yl)-1H-pyrazol-1-yl] ethanaminedihydrochloride (50 g, 0.16 mol), 5-methyl-2-(2H-1,2,3-triazol-2-yl)benzoic acid (33.9 g, 0.18 mol), 1-hydroxy-1H-benzotriazolehydrate (HOBtH2O) (26.4 g, 0.20 mol) and triethylamine (TEA)(39.5 g, 0.39 mol) in THF (500 mL) at 0 C, followed by stirring atroom temperature for 20.5 h. The solvent of the reaction solutionwas distilled off under reduced pressure. An aqueous NaHCO3 solutionand EtOAc were added to the resulting residue, followed byextraction with EtOAc. The organic layer was washed with water,and the solvent was distilled off under reduced pressure to yieldthe crude product (72 g). An additional 196.7 g of the crude productwas synthesized using the same method from N-ethyl-2[3-(5-fluoro-pyridin-2-yl)-1H-pyrazol-1-yl] ethanamine dihydrochloride(140 g, 0.46 mol) and 5-methyl-2-(2H-1,2,3-triazol-2-yl)benzoicacid (94.8 g, 0.50 mol). The obtained crude product (268.7 g) wasrecrystallized with heptane and EtOAc. The deposited solid wasthen collected by filtration. The obtained solid was dried by heatingunder reduced pressure to yield the title compound 27e as acolorless powder (217.3 g).

The potential utility of systematic synthetic strategy will be applicable to efficient generations of chemical libraries of compounds to find ‘hit’ molecules.Read on for other articles about 5-Methyl-2-(2H-1,2,3-triazol-2-yl)benzoic acid, hurry up and to see.

Reference:
Article; Suzuki, Ryo; Nozawa, Dai; Futamura, Aya; Nishikawa-Shimono, Rie; Abe, Masahito; Hattori, Nobutaka; Ohta, Hiroshi; Araki, Yuko; Kambe, Daiji; Ohmichi, Mari; Tokura, Seiken; Aoki, Takeshi; Ohtake, Norikazu; Kawamoto, Hiroshi; Bioorganic and Medicinal Chemistry; vol. 23; 6; (2015); p. 1260 – 1275;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Research speed reading in 2021. Redox catalysis has been broadly utilized in electrochemical synthesis due to its kinetic advantages over direct electrolysis. 61-82-5, name is 1H-1,2,4-Triazol-5-amine belongs to triazoles compound, it is a common compound, a new synthetic route is introduced below. 61-82-5

General procedure: A mixture of aldehyde (1.0 mmol), dimedone (1.0 mmol),1H-1,2,4-triazol-3-amine (1.0 mmol) and nano-AlPO4(SO3H) (0.1 g) was stirred in the acetonitrile (4.0 mL)at 50 C for an appropriate time. After the completion of thereaction as indicated by TLC, dichloromethane was addedto the solidified mixture and the insoluble catalyst was separatedby centrifugation. Evaporation of the solvent from thefiltrate and recrystallization of the solid residue from hot ethanolafforded the pure products in good to excellent yields

Balanced chemical reaction does not necessarily reveal either the individual elementary reactions by which a reaction occurs or its rate law. In my other articles, you can also check out more blogs about 61-82-5, and we look forward to future research findings.

Reference:
Article; Sharghi, Hashem; Aboonajmi, Jasem; Aberi, Mahdi; Shiri, Pezhman; Journal of the Iranian Chemical Society; vol. 15; 5; (2018); p. 1107 – 1118;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Research speed reading in 2021. In classical electrochemical theory, both the electron transfer rate and the adsorption of reactants at the electrode control the electrochemical reaction. 288-36-8, name is 1H-1,2,3-Triazole belongs to triazoles compound, it is a common compound, a new synthetic route is introduced below. Safety of 1H-1,2,3-Triazole

In a round-bottomed flask equipped with an overhead magnetic stirrer, reflux condenser, and nitrogen inlet were added 5-chloro-2-iodobenzoic acid (1 .15 g, 4.07 mmol), copper iodide (0.04 g, 0.2 mmol), and CS2CO3 (2.65 g, 8.14 mmol). To these solids were added dioxane (6 mL), water (0.05 mL), then 1 H-1 ,2,3-triazole (0.47 mL, 8.14 mmol), and finally trans-1 ,2-dimethylcyclohexane-1 ,2-diamine (0.3 mL, 0.81 mmol). The mixture was then warmed to 100 C for 4 hrs. Then the mixture was cooled and then MTBE and of water were added. After vigorous mixing, the layers were separated and the bottom aqueous layer was acidified to pH 2 with 6N HCI. The aqueous was then extracted twice with EtOAc. The combined organic layers were dried, filtered, and concentrated. The oil was stirred overnight in EtOAc (8 mL) and the resulting precipitate was removed by filtration affording a first crop of wanted product(100 mg). The mother-liquors were concentrated and purified by FC on S1O2 column (eluting from DCM to DCM : MeOH: 90: 10) to afford a second batch of the desired product that was mixed with the former to afford 5-chloro-2-(2H-1 ,2,3-triazol-2- yl)benzoic acid (p120, 620 mg, y=68%). MS (mlz): 223.9 [MH]+

Sometimes chemists are able to propose two or more mechanisms that are consistent with the available data. If a proposed mechanism predicts the wrong experimental rate law, however, the mechanism must be incorrect.Welcome to check out more blogs about 1H-1,2,3-Triazole, in my other articles.

Reference:
Patent; CHRONOS THERAPEUTICS LIMITED; MICHELI, Fabrizio; BERTANI, Barbara; GIBSON, Karl Richard; DI FABIO, Romano; RAVEGLIA, Luca; ZANALETTI, Riccardo; CREMONESI, Susanna; POZZAN, Alfonso; SEMERARO, Teresa; TARSI, Luca; LUKER, Timothy Jon; (275 pag.)WO2019/43407; (2019); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

New discoveries in chemical research and development 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. 956317-36-5, name is 5-Methyl-2-(2H-1,2,3-triazol-2-yl)benzoic acid belongs to triazoles compound, it is a common compound, a new synthetic route is introduced below. name: 5-Methyl-2-(2H-1,2,3-triazol-2-yl)benzoic acid

HOBt.H2O (1.1 g, 7.4 mmol) and EDC.HCl (1.4 g, 7.4 mmol) were added to a solution of 3,3-diethoxypropan-1-amine (0.96 mL, 5.9 mmol) and 5-methyl-2-(2H-1,2,3-triazol-2-yl)benzoic acid (1.0 g, 4.9 mmol) in DMF (18 mL), followed by stirring at room temperature for 3 hours. An aqueous NaHCO3 solution was added to the reaction solution, followed by extraction with EtOAc. The organic layer was washed with water and brine and was dried with Na2SO4. The desiccant was then removed by filtration, and the solvent was distilled off under reduced pressure. The resulting residue was purified by column chromatography (KP-Sil: 25 g, hexane/EtOAc=85/15 to 0/100) to give the titled compound (1.6 g, colorless solid). MS (ESI pos.) m/z: 333 [M+H]+

If you are hungry for even more, make sure to check my other article about 956317-36-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; TAISHO PHARMACEUTICAL CO., LTD.; Suzuki, Ryo; Futamura, Aya; Abe, Masahito; Kashiwa, Shuhei; Hattori, Nobutaka; Nozawa, Dai; Ohta, Hiroshi; Araki, Yuko; US2014/81025; (2014); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Synthetic Route of 217448-86-7, New Advances in Chemical Research in 2021. As an important bridge between the micro and macro material world, chemistry is one of the main methods and means for humans to understand and transform the material world. 217448-86-7, name is Methyl 1-(2,6-difluorobenzyl)-1H-1,2,3-triazole-4-carboxylate, molecular formula is C11H9F2N3O2, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, below Introduce a new synthetic route.

General procedure: A 250 mL two-necked round bottomflask was charged with sodium azide (6.10 g, 93.8 mmol), compound2 (1.90 g, 6.84 mmol), and water (20 mL). After the solidwas completely dissolved, compound 1a (5.0 g, 31.37 mmol) andCH3CN (80 mL) were added. The mixture was stirred at room temperaturefor 3 h, and then the CH3CN layer was separated. To theCH3CN solution were added Cu2O-NP (0.42 g) and compound 4(2.80 mL, 31.3 mmol), and the reaction mixture was stirred for8 h at room temperature under protection of inert gas. The mixturewas filtered and the filtrate was concentrated, and was chargedwith methanol (40 mL) and 35% ammonia in water (100 mL). The mixture was heated to 65 C and refluxed for 4 h, cooled to roomtemperature, and filtered. The resulting solid was washed withwater and methanol to obtain rufinamide (5.25 g, 71.6%) as colorlesscrystalline product. Mp: 242-244 C. 1H NMR (400 MHz,DMSO-d6) d 8.549 (s, 1H), 7.842 (br s, 1H), 7.566-7.470 (m, 2H),7.215-7.174 (m, 2H), 5.723 (s, 2H). 13C NMR (100 MHz, DMSOd6)d 162.5, 161.7, 160.0, 143.3, 132.3, 127.4, 112.4, 111.5, 41.66.MS (ESI+): 239.06.

The potential utility of systematic synthetic strategy will be applicable to efficient generations of chemical libraries of compounds to find ‘hit’ molecules.Read on for other articles about Methyl 1-(2,6-difluorobenzyl)-1H-1,2,3-triazole-4-carboxylate, hurry up and to see.

Reference:
Article; Wang, Jing-Han; Pan, Cheng-Wen; Li, Yong-Tao; Meng, Fan-Fei; Zhou, Hong-Gang; Yang, Cheng; Zhang, Quan; Bai, Cui-Gai; Chen, Yue; Tetrahedron Letters; vol. 54; 26; (2013); p. 3406 – 3409;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Related Products of 3641-08-5, New discoveries in chemical research and development in 2021. We’ll be discussing some of the latest developments in chemical about CAS: 3641-08-5, name is 2H-1,2,4-Triazole-3-carboxamide, 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.

EXAMPLE 10 Preparation of 1(and 2 and 4)-Pivaloyl-s-triazole-3-carboxamide To a cooled, stirred mixture of 3 g. of 1,2,4-triazole-3-carboxamide and 3.4 g. of pivaloyl chloride in 125 ml. of anhydrous diethyl ether is added rapidly 2.75 g. of triethylamine. The cooling bath is removed and the mixture is stirred at room temperature for 24 hours. The off-white solid is collected by filtration and washed thoroughly with diethyl ether and then cold water.

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 2H-1,2,4-Triazole-3-carboxamide.

Reference:
Patent; American Cyanamid Company; US4006159; (1977); A;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Related Products of 16681-65-5, New Advances in Chemical Research in 2021.In classical electrochemical theory, both the electron transfer rate and the adsorption of reactants at the electrode control the electrochemical reaction. 16681-65-5, name is 1-Methyl-1H-1,2,3-triazole, molecular formula is C3H5N3, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, below Introduce a new synthetic route.

1-Methyl-1H-1,2,3-triazole was prepared according to the literature reference WO2008/98104. To a 2 L flask containing 1-methyl-1H-1,2,3-triazole (9 g, 108.3 mmol) was added THF (1500 mL) and the solution was cooled to -40 C. To this colorless homogeneous solution was added n-butyllithium (2.5 M in hexanes, 45 mL, 112.5 mmol) dropwise which immediately afforded a dark brown viscous mixture. The mixture was kept between -10 to -20 C. for 60 minutes, then a THF solution of 2,4-dimethylthiazole-5-carbaldehyde (17.2 g, 121.8 mmol in 200 mL THF) was introduced via cannula. Once the aldehyde was added the reaction was allowed to warm to room temperature. After 3 hours, the reaction was quenched by pouring into a saturated solution of aqueous NH4Cl. The aqueous portion was extracted with EtOAc in portions, 7*400 mL. The combined organics were washed with brine, dried over MgSO4, filtered and concentrated to give a brown oil. Chromatography on silica gel (10% acetone-DCM increasing to 50% acetone and increasing to 10% MeOH-DCM) provided the title compound as an amber solid.

Future efforts will undeniably focus on the diversification of the new catalytic transformations. These may comprise an expansion of the substrate scope from aromatic and heteroaromatic compounds to other hydrocarbons. Keep reading other articles of 16681-65-5.

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.; Jones, William Moore; Goldberg, Steven; US2015/105366; (2015); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Electric Literature of 4928-87-4, New discoveries in chemical research and development in 2021. We’ll be discussing some of the latest developments in chemical about CAS: 4928-87-4, name is 1,2,4-Triazole-3-carboxylic acid, 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.

Single crystals of 1 were prepared by a branched tube method [13], 1H-1,2,4-triazole-3-carboxylic acid (0.117 g, 1 mmol), lead(II) nitrate (0.331 g, 1 mmol) and potassium bromide (0.119 g, 1 mmol) were placed in the bottom main of a branched tube. Water was carefully added to fill both arms, and then the arm to be heated was placed in oil bath at 60 C. After 3 days, colorless crystals were deposited in the cooler arm which were filtered off, washed with water and air dried. (0.225 g, yield 54%), m.p. ?195 C. (Found C 8.55, H 0.99, N 10.43%. calculated for C3H4BrN3O3Pb; C 8.63, H 0.96, N 10.07%). IR (cm-1) selected bands: 464 (s), 651 (s), 1100 (s), 1303 (m), 1370 (m), 1457 (vs), 1606 (s) and 3370 (br).

The potential utility of systematic synthetic strategy will be applicable to efficient generations of chemical libraries of compounds to find ‘hit’ molecules.Read on for other articles about 1,2,4-Triazole-3-carboxylic acid, hurry up and to see.

Reference:
Article; Safarifard, Vahid; Morsali, Ali; Joo, Sang Woo; Ultrasonics Sonochemistry; vol. 20; 5; (2013); p. 1254 – 1260;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics