Tag: M.W=0-100

16681-65-5, name is 1-Methyl-1H-1,2,3-triazole, belongs to Triazoles compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Recommanded Product: 16681-65-5

To a flask containing 1-methyl-1H-1,2,3-triazole (125 mg, 1.5 mmol) was added THF (10 mL) and the colorless solution was cooled to -45 C. Then, n-BuLi (2.5 M in hexanes, 0.6 mL, 1.5 mmol) was added affording a suspension. The suspension was stirred between -40 C. and -10 C. for 30 minutes, then a THF solution of (2,4-dichloro-3-phenylquinolin-6-yl)(1,2-dimethyl-1H-imidazol-5-yl)methanone (500 mg, 1.26 mmol, Intermediate 18: step b, in 5 mL THF) was introduced and the mixture was allowed to warm up to room temperature. After 1 hour, the reaction mixture was heated to 40 C. for 3 hours and then quenched with aqueous NH4Cl solution. The aqueous portion was extracted with EtOAc (3*50 mL) and then with DCM (3*50 mL). The individual organic portions were washed with brine, dried over MgSO4, filtered, combined and concentrated to dryness. Chromatography on silica gel (5% MeOH-DCM increasing to 10% MeOH) provided material which was re-purified by preparative TLC (5% 2 M-NH3-MeOH-EtOAc) to provide the title compound as light tan solid. 1H NMR (500 MHz, CDCl3) delta 8.45-8.36 (m, 1H), 7.94 (d, J=8.8 Hz, 1H), 7.66-7.46 (m, 4H), 7.46-7.30 (m, 2H), 7.01 (s, 1H), 5.94 (s, 1H), 3.91 (s, 3H), 3.34 (s, 3H), 2.17 (s, 3H). MS (ESI): mass calcd. for C24H20Cl2N6O, 478.1, m/z found 479.1 [M+H]+.

The synthetic route of 16681-65-5 has been constantly updated, and we look forward to future research findings.

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.; US2015/105404; (2015); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Synthetic Route of 288-36-8, The chemical industry reduces the impact on the environment during synthesis 288-36-8, name is 1H-1,2,3-Triazole, I believe this compound will play a more active role in future production and life.

1,2,3-triazole (3.45 g, 50 mmol), 2-iodo-5-methylbenzoic acid (5.24 g, 20 mmol), cesium carbonate (0.57 g, 3.6 mmol), cuprous iodide (0.38 g, 2 mmol), trans-N, N’-dimethyl-1,2-cyclohexanediamine (0.51 g, 3.6 mmol), N, N-dimethylformamide (30 mL)was added sequentially to a 100 mL single-necked round bottom flask and gradually heated under nitrogen to 100 C for 4 hours. The reaction was quenched, cooled, diluted with tap water and washed with ethyl acetate (200 mL x 2). The aqueous layer was acidified with concentrated hydrochloric acid (pH = 1~2) and extracted with ethyl acetate (200 mL x 2). The organic layers were combined and dried over anhydrous sodium sulfate. The filtrate was evaporated under reduced pressure and purified by column chromatography (dichloromethane / methanol (v/v) = 50/1) to give the title compound (yellow solid, 2.76 g, 68%).

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, 1H-1,2,3-Triazole, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Guangdong Dongyangguang Pharmaceutical Co., Ltd.; Dongguan Dongyangguang Pharmaceutical Research And Development Co., Ltd.; Jin Chuanfei; Du Changfeng; Zhang Yingjun; Liu Yanping; Kou Yuhui; (38 pag.)CN106986859; (2017); A;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Electric Literature of 1455-77-2, 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. 1455-77-2 name is 3,5-Diamino-1,2,4-triazole, 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.

The reaction mixture for the synthesis of new class II hybridfluorinated is formed by two metal cations in fluorinated forms FeF2and FeF3, an aqueous solution of hydrofluoric acid 4percent (prepared from40percent HF, Riede-deHaen), a solvent such as ethanol, which is polar andprotic, and with a cyclic organic molecule (3,5-diamino-1,2,4-triazole).The solvent volume was fixed to 10 mL with a constant concentration[FeII] + [FeIII] = 0.15 mol L?1 and an equimolar ratio n(FeII)/n(FeIII)= 1. Indeed, [Fe3F8(H2O)2](Am2TAZ)2 is obtained from a mixture of85 mg of FeF3 (0.75 mmol), 70 mg of FeF2 (0.75 mmol), 2.52 mL of HF2.3M (5.8 mmol) and 57 mg (Am2TAZ) (0.57 mmol).The starting materials were placed in a reactor when filling 50percent ofthe autoclave. After manipulation, the solid product is washed with thesolvent used, then air dried at room temperature. As a result, a newmixed hybrid fluoride was obtained. Therefore, the exploration of thissystem FeF2/ FeF3 – HF – (Am2TAZ) ? EtOH, led by hydrothermalsynthesis at 120 ¡ãC for 72 h, yielded to the elaboration of a new phaseof formula [Fe3F8(H2O)2](Am2TAZ)2 colorless with prismatic shape.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3,5-Diamino-1,2,4-triazole, and friends who are interested can also refer to it.

Reference:
Article; Bouketaya, Sabrine; Smida, Mouna; Abdelbaky, Mohammed S.M.; Dammak, Mohamed; Garcia-Granda, Santiago; Journal of Solid State Chemistry; vol. 262; (2018); p. 343 – 350;,
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. 288-88-0, name is 1H-1,2,4-Triazole belongs to Triazoles compound, it is a common compound, a new synthetic route is introduced below. name: 1H-1,2,4-Triazole

0.69 g (10 mmol) of 1,2,4-triazole and 2.07 g (15 mmol) of potassium carbonate were weighed.1.24 g (10 mmol) of p-fluorobenzaldehyde,It was dissolved in 20 mL of N,N-dimethylformamide, and added to a 100 mL three-necked flask equipped with a thermometer and a stirring apparatus.The reaction was carried out under constant temperature stirring at 100C for 16 h, cooled to room temperature, extracted, suction filtered, separated by column chromatography, washed with warm water, recrystallized from anhydrous ethanol, and dried under vacuum at 50C for 8h that is, 1,2,4-triazole benzaldehyde.

The synthetic route of 288-88-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Qilu University of Technology; Duan Hongdong; Zhong Wenxia; Wang Lizhen; (12 pag.)CN109761992; (2019); A;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Related Products of 16681-65-5, These common heterocyclic compound, 16681-65-5, name is 1-Methyl-1H-1,2,3-triazole, 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.

To a 2-necked flask containing 1 -methyl-1 H-[1 ,2,3]triazole (162.91 mg; 1.96 mmol; 1.05 eq.) is added anhydrous THF (4.00 ml_) and the solution is cooled between -40 to -20C. To this colorless solution n-BuLi in hexane 1 .6M (1 .23 ml; 1 .96 mmol; 1 .05 eq.) is added dropwise. After stirring at 0C for 1 hour, a solution of pyridine-3-carbaldehyde (175.28 L; 1.87 mmol; 1 .00 eq.) in anhydrous THF (3.00 mL) is added and the reaction mixture is stirred for 3 h. After this time, RM is quenched by pouring into a saturated solution of NH4CI. Aqueous phase is extracted 3 times with n-BuOH. Organic layer is dried over Na2S04, filtered and concentrated in vacuo to obtain: (3-methyl- 3H-[1 ,2,3]triazol-4-yl)-pyridin-3-yl-methanol (243.00 mg; yield 66 %; 99 % by UPLC) is obtained as a beige oil.

The synthetic route of 16681-65-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SELVITA S.A.; FABRITIUS, Charles-Henry Robert Yves; NOWAK, Mateusz Oktawian; WIKLIK, Katarzyna Anna; SABINIARZ, Aleksandra Barbara; BIE?, Marcin Dominik; BUDA, Anna Ma?gorzata; GUZIK, Pawel Szczepan; JAKUBIEC, Krzysztof Roman; MACIUSZEK, Monika; KWIECI?SKA, Katarzyna; TOMCZYK, Mateusz Micha?; GA??ZOWSKI, Micha? Miko?aj; GONDELA, Andrzej; DUDEK, ?ukasz Piotr; (681 pag.)WO2016/180536; (2016); 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. 1455-77-2, name is 3,5-Diamino-1,2,4-triazole, This compound has unique chemical properties. The synthetic route is as follows., Formula: C2H5N5

A suspension of 1H-1,2,4-triazole-3,5-diamine (1.98 g, 20 mmol) in EtOH (80 mL) was treated with 1-phenyl-1H-pyrazole-4-carbaldehyde-hydrate (3.52 g, 20 mmol) and the resulting mixture heated at reflux for 3 h. The mixture was cooled to rt and NaBH4 (832 mg, 22.0 mmol) was added portion-wise. The reaction mixture reheated to 40 ¡ãC for 15 minutes. The solvent of the mixture was then evaporated to ~ half volume, the solids filtered, and the collected precipitate was air dried to afford the title compound as a colorless solid (2.45 g, 48percent). 1H NMR (400MHz, DMSO-d6) delta = 10.78 (br s, 1H), 8.33 (s, 1H), 7.77 (d, J = 1.2 Hz, 1H), 7.76 – 7.74 (m, 1H), 7.67 (s, 1H), 7.47 (dd, J = 7.6, 8.4 Hz, 2H), 7.31 – 7.24 (m, 1H), 5.82 (br s, 1H), 5.34 (br s, 2H), 4.14 (d, J = 6.3 Hz, 2H); [M+H] = 256.22.

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 1455-77-2.

Reference:
Patent; DART NEUROSCIENCE, LLC; ALLAN, Amy, Lynn; BREITENBUCHER, James; GOMEZ, Laurent; KEENAN, Terence, Patrick; LEMUS, Robert; LY, Kiev; MARRONE, Tami, Jo; (119 pag.)WO2016/73424; (2016); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Related Products of 16681-65-5, A common heterocyclic compound, 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, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

A 50 mL flask containing 1-methyl-1H-1,2,3-triazole (0.47 g, 5.71 mmol) in dry THF (3 mL) was cooled to -43 C. (CH3CN-CO2 bath). n-Butyllithium (2.5 M in THF, 2.43 mL, 6.08 mmol) was then added dropwise resulting in a light blue suspension. The suspension was stirred at -40 C. for 40 minutes, and then a homogeneous solution of 6-(trifluoromethyl)nicotinaldehyde (1 g, 5.71 mmol) in THF (7 mL) was introduced at -40 C. The resulting homogeneous colorless solution was allowed to warm gradually to room temperature, and after 30 minutes, LC/MS showed that the reaction was complete. The mixture was quenched with water and aqueous NH4Cl and extracted with EtOAc (2*). The combined organic extracts were washed with brine, dried over Na2SO4, filtered and concentrated to provide the title compound as a semi-solid which was carried on to the next step without further purification.

The synthetic route of 16681-65-5 has been constantly updated, and we look forward to future research findings.

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

Reference of 16681-65-5, 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. 16681-65-5, name is 1-Methyl-1H-1,2,3-triazole belongs to Triazoles compound, it is a common compound, a new synthetic route is introduced below.

To a flask containing 1-methyl-1H-1,2,3-triazole (275 mg, 3.31 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, 1.4 mL, 3.5 mmol) was added dropwise which afforded an opaque white suspension. The mixture was stirred at -43 C. for 20 minutes, then a homogeneous solution of (4-chloro-3-isobutyl-2-methoxyquinolin-6-yl)(1,2-dimethyl-1H-imidazol-5-yl)methanone (550 mg, 1.48 mmol, Intermediate 65) in 3 mL THF was introduced. After 10 minutes, the reaction flask was then placed in an ice-water bath. The reaction mixture was quenched after 30 minutes with aqueous NH4Cl solution and the aqueous portion was extracted with EtOAc (4*30 mL) and EtOAc:THF (1:1, 30 mL). The combined organics were washed with brine, dried over MgSO4, filtered and concentrated. Chromatography on silica gel (5% MeOH-DCM increasing to 10% MeOH-DCM) provided the title compound as a tan amorphous solid. 1H NMR (400 MHz, CD3OD) delta 8.19 (d, J=2.1 Hz, 1H), 7.85 (d, J=8.7 Hz, 1H), 7.52 (dd, J=8.7, 2.2 Hz, 1H), 7.17 (s, 1H), 6.11 (s, 1H), 4.09 (s, 3H), 3.98 (s, 3H), 3.47 (s, 3H), 2.85 (d, J=7.3 Hz, 2H), 2.37 (s, 3H), 2.11 (hept, J=6.9 Hz, 1H), 0.96 (d, J=6.6 Hz, 6H). MS (ESI): mass calcd. for C23H27ClN6O2, 454.2. m/z found 455.0 [M+H]+. The racemate was separated by chiral SFC (Stationary phase: CHIRALPAK AD-H 5 mum, 250¡Á30 mm, Mobile phase: 70% CO2, 30% mixture of MeOH/iPrOH 50/50 v/v (+0.3% iPrNH2)), to give Example 134b as the first compound that eluted from the chiral column and Example 134c as the second compound that eluted from the chiral column.

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

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

Adding a certain compound to certain chemical reactions, such as: 1455-77-2, name is 3,5-Diamino-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 1455-77-2, COA of Formula: C2H5N5

General procedure: An equimolar solution of 3,5-diamino-1,2,4-triazole (0.99?g, 0.01?mol) and 2-hydroxynaphthaldehyde (1.72?g, 0.01?mol) in dry methanol (50?mL) was refluxed for 3?h, a precipitated product was formed during refluxing. It was then cooled to room temperature, filtered, washed with methanol (35?mL), then with diethyl ether (2?¡Á?5?mL) and dried under vacuum. Recrystallization in a mixture of methanol:dioxane (1:4) gave TLC pure product (L1) in 83percent yield. The same method was applied for the preparation of all other ligands (L2)?(L5).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3,5-Diamino-1,2,4-triazole, and friends who are interested can also refer to it.

Reference:
Article; Sumrra, Sajjad H.; Chohan, Zahid H.; Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy; vol. 98; (2012); p. 53 – 61;,
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. 1455-77-2, name is 3,5-Diamino-1,2,4-triazole, A new synthetic method of this compound is introduced below., Computed Properties of C2H5N5

A solution of 3-(dimethylamino)-1-phenylpropan-1-one hydrochloride 9 (9.36 mmol) and diaminotriazole 10 (9.36 mmol) in 20 mL of acetic acid was heated to reflux for 6 h. The reaction mixture was cooled and the solvent evaporated in vacuo to furnish a mixture of desired product 12 (minor) and 5-phenyl-6,7-dihydro-[1,2,4]triazolo[1,5-a]pyrimidin-2-amine (major). The crude mixture was taken to the next step without any further purification and it was treated with N-bromosuccinimide (14.03 mmol) in ethanol (20 mL) under reflux for 5 h to promote the oxidation of the dihydrotriazolopyrimidine. The reaction mixture was cooled, and the solvent was evaporated in vacuo to yield a pale-yellow solid. The crude compound was purified by flash chromatography on silica gel using as eluent a gradient of EtOAc (0-50percent) to produce the desired compound 12 as white solid (adapted from 2). Yield: 29percent (0.57 g). 1H NMR (600 MHz, DMSO-d6) delta 9.07 (d, J = 6.9 Hz, 1H), 8.21 ? 8.19 (m, 2H), 7.72 (d, J = 6.9 Hz, 1H), 7.56 (s, 3H). HRMS-ESI (+) m/z calculated for C11H10N5, 212.0936 [M+H]+; found: 212.0941

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

Reference:
Article; Ribeiro, Carlos J.A.; Kankanala, Jayakanth; Xie, Jiashu; Williams, Jessica; Aihara, Hideki; Wang, Zhengqiang; Bioorganic and Medicinal Chemistry Letters; vol. 29; 2; (2019); p. 257 – 261;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics