Tag: M.W=0-100

Related Products of 41253-21-8, The chemical industry reduces the impact on the environment during synthesis 41253-21-8, name is Sodium 1,2,4-triazol-1-ide, I believe this compound will play a more active role in future production and life.

To a solution of 2,4-difluorobenzonitrile (10 g, 72 mmol) dissolved in THF (20 mL), and DMF (40 mL) was added 1,2,4-triazole sodium derivative (6.3 g, 70 mmol) and the mixture was stirred at 90 C. for 3 h, filtered and concentrated. The residue was adsorbed onto Silica gel and purified by flash chromatography eluting with 0%-10%-30% EtOAc/hexanes to give intermediate 1 as colorless needles (2.46 g, 18%) and intermediate 2 was obtained as a white solid (0.7455 g, 6%). Intermediate 1 4-Fluoro-2-(1H-1,2,4-triazol-1-yl)benzonitrile: 1H NMR (500 MHz, CDCl3) delta: 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. Intermediate 2 4-(1H-1,2,4-triazol-1-yl)-2-fluorobenzonitrile: 1H NMR (500 MHz, CDCl3) delta: 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.

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; Bristol-Myers Squibb Company; US2007/112190; (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. 60166-43-0, name is 1,4-Dimethyl-1H-1,2,3-triazole, A new synthetic method of this compound is introduced below., COA of Formula: C4H7N3

In a 75 mL pressure vessel equipped with a magnetic stirring bar, was added (5)- 3-bromo-7-chloro-5-((2-fluorophenyl)(tetrahydro-2H-pyran-4-yl)methyl)-5H-pyrrolo[2,3- b:4,5-b’]dipyridine (650 mg, 1.37 mmol), l,4-dimethyl-lH-l,2,3-triazole (199 mg, 2.05 mmol) and NMP (10 mL). Tetramethyl NH4OAC (274 mg, 2.05 mmol) and bis(triphenylphosphine) palladium(II) chloride (67.3 mg, 0.096 mmol) was added. Argon was bubbled into the mixture with sonication for 5 min, then the vessel was capped and placed into a preheated oil bath at 100C. The reaction mixture was stirred overnight. Most of the solvent was removed under a stream of nitrogen while heating for several hours in an oil bath set at 100C. The remaining mixture was taken up in 2 mL of DMF then filtered for purification by preparative HPLC: Column: Waters XBridge CI 8, 19 x 200 mm, 5-muiotatauiota particles; Mobile Phase A: 5:95 methanol: water with lOmM NLUOAc; Mobile Phase B: 95:5 methanol: water with lOmM NHtOAc; Gradient: 10-80% B over 30 min, then a 5-min hold at 100% B; Flow: 20 mL/min. Fractions containing the desired product were combined and dried via centrifugal evaporation to give 4.7 mg (0.6%) of the title compound with an average purity by LC/MS analysis was >99%. Two analytical LC/MS injections were used to determine the final purity. Injection 1 conditions: Column: Waters BEH C18, 2.0 x 50 mm, 1.7um particles; Mobile Phase A: 5:95 ACN:water with 10 mM NH4OAc; Mobile Phase B: 95:5 ACN:water with 10 mM NH4OAc; Temperature: 50C; Gradient: 0%B, 0-100% B over 3 min, then a 0.5-min hold at 100% B; Flow: 1 mL/min; Detection: UV at 220 nm. Rt= 1.50 min; LC/MS (M+H) = 552.5. Injection 2 conditions: Column: Waters BEH C18, 2.0 x 50 mm, 1.7-mupiiota particles; Mobile Phase A: 5:95 methanol: water with 10 mM NFL Ac; Mobile Phase B: 95:5 methanol: water with 10 mM NH4OAc; Temperature: 50C; Gradient: 0%B, 0-100% B over 3 min, then a 0.5-min hold at 100% B; Flow: 0.5 mL/min; Detection: UV at 220 nm. Rt= 2.51 min; LC/MS (M+H) = 552.5. NMR (500MHz, DMSO-c e) delta 8.81 (d, J=8.1 Hz, 1H), 8.68 (s, 1H), 8.46 (br. s., 1H), 8.20 (br. s., 1H), 7.71 (d, J=8.1 Hz, 1H), 7.34 (d, J=5.5 Hz, 1H), 7.29 (d, J=7.7 Hz, 1H), 7.17 – 7.04 (m, 1H), 6.36 (br. s., 1H), 4.34 (br. s., 3H), 4.00 (br. s., 3H), 3.93 – 3.83 (m, 1H), 3.72 (d, J=9.5 Hz, 1H), 3.47 – 3.38 (m, 4H), 3.27 – 3.15 (m, 1H), 2.29 (br. s., 3H), 1.72 (d, J=11.7 Hz, 1H), 1.58 – 1.42 (m, 1H), 1.33 (d, J=12.1 Hz, 1H), 0.98 (d, J=13.2 Hz, 1H). LC/MS (M+H) = 552.5; HPLC conditions: Rt= 2.57 min (Phenomenex LUNA C18 2 x 50 mm (4 min grad) eluting with 5-95% aq ACN containing lOmM NH4OAC, 0.8 mL/min, monitoring at 254 nm); Temperature: 40C).

The synthetic route of 60166-43-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; NORRIS, Derek J.; VACCARO, Wayne; DEBENEDETTO, Mikkel V.; DEGNAN, Andrew P.; DELUCCA, George V.; DESKUS, Jeffrey A.; HAN, Wen-Ching; KUMI, Godwin Kwame; SCHMITZ, William D.; STARRETT, John E., JR.; HILL, Matthew D.; HUANG, Hong; (563 pag.)WO2016/183118; (2016); 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. COA of Formula: C2H2N3Na

a stirrer after replacement with nitrogen,Add the thermometer and condenser to the reaction bottle1-(4-chlorophenyl)-4,4-dimethyl-3-butanone100g,Trimethyl thionyl chloride 63g,28 g of potassium hydroxide and 100 g of dimethyl sulfoxide (DMSO) and stirred.After 40 C reaction to 1 – (4 – chlorophenyl) – 4,4 – dimethyl -3 – pentanone reaction,Add sodium triazole sodium 60g, react at 120 C,After the reaction, desolvation, add 100 g of methylcyclohexane, and wash with 30 g of water.Layering at 70 C, recrystallization from water at 25 C,After suction filtration, the mixture was dried to obtain 130 g of tebuconazole, the yield was 91%, and the purity was 96%.

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; Jiangsu Qi Zhou Green Chemical Co., Ltd.; Wu Tianyu; Liu Yuchao; Tao Yachun; Cai Junyi; Wang Hai; (6 pag.)CN109336848; (2019); A;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 7170-01-6, name is 3-Methyl-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 7170-01-6, Quality Control of 3-Methyl-1H-1,2,4-triazole

2,3-Dichloro-5-nitropyridine (2 g, 10.36 mmol), 3-methyl-1H-1,2,4-triazole (1.722 g, 20.73 mmol) and Cs2CO3 (6.798 g, 20.73 mmol) were added to DMF (30 mL) and the reaction was stirred at rt for 12 h. The reaction mixture was quenched with water (200 mL). The mixture was extracted with ethyl acetate (100 mL*3). The organic layer was dried over Na2SO4, filtered, and the filtrate concentrated under reduced pressure. The crude residue was purified by flash column chromatography over silica gel (petroleum ether/ethyl acetate from 100:0 to 50:50) to afford a mixture of compounds 20a and 20a-1 (780 mg, 31%) as a white solid.

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

Reference:
Patent; Janssen Biotech, Inc.; Lu, Tianbao; Allison, Brett Douglas; Barbay, Joseph Kent; Connolly, Peter J.; Cummings, Maxwell David; Diels, Gaston; Edwards, James Patrick; Kreutter, Kevin D.; Philippar, Ulrike; Shen, Fang; Thuring, Johannes Wilhelmus John Fitzgerald; Wu, Tongfei; (412 pag.)US2018/170909; (2018); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Reference of 288-36-8, A common heterocyclic compound, 288-36-8, name is 1H-1,2,3-Triazole, molecular formula is C2H3N3, 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.

1- (3-CHLORO-PROPOXY)-4-NITRO-BENZENE (7 g, 32.5 mmol) is dissolved in 2-methyl- 2-butanol (35 ml) followed by the addition of 1H-1, 2,3-triazole (3.43 g, 48.7 mmol), potassium iodide (0.54 g, 3.25 mmol) and sodium hydroxide (1.95 g, 48.7 mmol). The mixture is stirred for 20 h at 120 C, evaporated to dryness and suspended in toluene. Washing with water, drying over sodium sulfate and concentration in vacuo yields a crude product, which is washed with ether yielding L- [3- (4-NITRO-PHENOXY)-PROPYL]-LH- [L, 2,3] triazole as a colorless solid. Yield 6 g (75 %) MS: M = 249.3 (API+) H-NMR (400 MHz, CDC13) : 2.48 (m, 2H), 4.07 (t, J = 5.77 Hz, 2H), 4.64 (t, J = 6.7 Hz, 2H), 6.93 (d, J = 9.3 Hz, 2H), 7.56 (s, 1H), 7.72 (s, 1H), 8.20 (d, J = 9.2 Hz, 2H).

The synthetic route of 288-36-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; WO2004/96796; (2004); 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. 288-36-8, name is 1H-1,2,3-Triazole, A new synthetic method of this compound is introduced below., category: Triazoles

Intermediate 6: 5-Methyl-2-(2H-1,2,3-triazol-2-yl)benzoic acid To a solution of 2H-1,2,3-triazole (CAS number 288-36-8; 1.99 g, 28.93 mmol) in DMF (7.0 ml) at 0-10 C. was added cesium carbonate (4.7 g, 14.45 mmol), trans-1-N,2-N-dimethylcyclohexane-1,2-diamine (0.127 g, 1.45 mmol), copper(I) iodide (0.068 g, 0.36 mmol) and 2-iodo-5-methylbenzoic acid (CAS number 52548-14-8; 3.79 g, 14.46 mmol). The reaction was subjected to microwave irradiation at 125 C. for 15 minutes, and then poured into water (20 ml) and extracted with ethyl acetate. The combined organics were washed with brine, dried over sodium sulfate and concentrated in vacuo. The crude product was purified by column chromatography (0-3% methanol/DCM) to afford the title compound. 1H NMR (DMSO-d6) delta ppm 2.42 (s, 3H), 7.49-7.52 (m, 1H), 7.58-7.64 (m, 2H), 8.05 (s, 2H), 13.01 (s, 1H). (0444) MS ES+: 204

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; Takeda Pharmaceutical Company Limited; Fieldhouse, Charlotte; Glen, Angela; Maine, Stephanie; Fujimoto, Tatsuhiko; Robinson, John Stephen; US2015/232460; (2015); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Related Products of 61-82-5, The chemical industry reduces the impact on the environment during synthesis 61-82-5, name is 1H-1,2,4-Triazol-5-amine, I believe this compound will play a more active role in future production and life.

General procedure: A mixture of aromaticaldehyde (1.0 mmol) and dimedone(1.0 mmol) with 2-aminobenzimidazole or 3-amino-1,2,4-triazole (1.0 mmol) was stirred in acetic acid (5 mL) at 60 Cfor the appropriate time (Tables 3, 4). The progress of thereaction was monitored by TLC. After completion of thereaction, a thick precipitate was obtained. The solid productwas filtered off and washed with acetic acid (3 × 2 mL) togive the pure products 4 and 6, and subsequently dried in air.The pure products were characterized by conventional spectroscopicmethods. Physical and spectral data for the compounds,4b, 4c, 4h, 4j, 6a, 6c, and 6h are represented below:

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-1,2,4-Triazol-5-amine, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Mousavi, Mir Rasul; Maghsoodlou, Malek Taher; Hazeri, Nourallah; Habibi-Khorassani, Sayyed Mostafa; Journal of the Iranian Chemical Society; vol. 12; 8; (2015); p. 1419 – 1424;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Synthetic Route of 288-36-8, 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. 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.

A solution of 2-bromo-3-thiophene carboxylic acid (1.50 g, 7.24 mmol), 1H-1,2,3- triazole (0.600 g, 8.69 mmol), potassium carbonate (2.00 g, 14.5 mmol), and copper iodide (0.138 g, 0.724 mmol) in DMF (36.2 mL) was purged subsurface with nitrogen and heated to 75 C for 96 h. The reaction was diluted with water, washed with ether, and acidified with cone. HC1. The acidic aqueous solution was extracted 3x with EtOAc and the combined organic fractions were washed with brine, dried over magnesium sulfate, filtered, and concentrated. The crude material was purified by silica gel gradient chromatography [0-70% (1% acetic acid in EtOAc) in hexanes], to provide Intermediate C as a solid. LRMS m/z (M+H) 196.2 found, 196.1 required.

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; MERCK SHARP & DOHME CORP.; KUDUK, Scott, D.; REGER, Thomas, S.; SKUDLAREK, Jason, W.; (0 pag.)WO2016/85784; (2016); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Application of 60166-43-0, The chemical industry reduces the impact on the environment during synthesis 60166-43-0, name is 1,4-Dimethyl-1H-1,2,3-triazole, I believe this compound will play a more active role in future production and life.

(R)-3-Bromo-7-chloro-5-(phenyl(tetrahydro-2H-pyran-4-yl)methyl)-5H- pyrrolo[2,3-b:4,5-b’]dipyridine (30.0 mg, 0.066 mmol), l,4-dimethyl-lH-l,2,3-triazole (25.5 mg, 0.263 mmol), Me4NOAc (21.8 mg, 0.164 mmol), and PdCl2(dppf)2.DCM (3.8 mg, 4.60 muetaiotaomicron) were weighed into a 20 mL scintillation vial, and 3 mL DMF was added and the air was replaced with nitrogen. The reaction mixture was heated to 100 C with stirring. After 1 h, it was cooled to room temperature, filtered, and concentrated. The crude material was purified via preparative LC/MS with the following conditions: Column: XBridge C18, 19 x 200 mm, 5-muiotaeta particles; Mobile Phase A: 5:95 ACN: water with 10-mM NH4OAc; Mobile Phase B: 95:5 ACN: water with 10-mM NH4OAc; Gradient: 20-60% B over 15 min, then a 5-min hold at 100% B; Flow: 20 mL/min. Fractions containing the desired product were combined and dried via centrifugal evaporation. The yield of the product was 4.2 mg, and its estimated purity by LC/MS analysis was 100%. Two analytical LC/MS injections were used to determine the final purity. Injection 1 conditions: Column: Waters BEH C18, 2.0 x 50 mm, 1.7-muetaiota particles; Mobile Phase A: 5:95 ACN:water with 10 mM NH4OAc; Mobile Phase B: 95:5 ACN:water with 10 mM NH4OAc; Temperature: 50 C; Gradient: 0%B, 0-100% B over 3 min, then a 0.5-min hold at 100% B; Flow: 1 mL/min; Detection: UV at 220 nm, RT = 1.52 min, LC/MS (M+H) = 534.5, LC/MS (M+H) = 534.5. Injection 2 conditions: Column: Waters BEH CI 8, 2.0 x 50 mm, 1.7-muiotaeta particles; Mobile Phase A: 5:95 methanol: water with 10 mM NH4OAc; Mobile Phase B: 95:5 methanol: water with 10 mM NH4OAc; Temperature: 50 C; Gradient: 0%B, 0-100% B over 3 min, then a 0.5-min hold at 100% B; Flow: 0.5 mL/min; Detection: UV at 220 nm. RT = 2.50 min, LC/MS (M+H) = 534.5. NMR (500MHz, DMSO-c e) delta 8.82 (d, J=8.1 Hz, 1H), 8.67 (s, 1H), 8.58 (br. s., 1H), 7.74 (t, J=7.2 Hz, 3H), 7.36 – 7.28 (m, 2H), 7.28 – 7.20 (m, 1H), 6.07 (br. s., 1H), 4.39 (s, 3H), 4.03 (s, 3H), 3.89 (d, J=13.6 Hz, 1H), 3.75 (d, J=9.9 Hz, 1H), 3.61 (br. s., 1H), 3.43 (t, .7=11.2 Hz, 1H), 3.24 (t, .7=11.4 Hz, 1H), 2.55 (s, 3H), 2.31 (s, 3H), 1.62 (br. s., 1H), 1.51 – 1.39 (m, 1H), 1.29 (d, J=8.4 Hz, 1H), 1.15 (br. s., 1H); LC/MS (M+H) = 534.3 [Column: Waters Aquity BEH C18 2.1 X 50 mm 1.7u; Mobile Phase A: water with 0.05% TFA; Mobile Phase B: ACN with 0.05% TFA; Temperature: 40 C; Gradient: 2-98% B over 1.5 min; Flow: 0.8 rnL/min].

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, 1,4-Dimethyl-1H-1,2,3-triazole, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; NORRIS, Derek J.; VACCARO, Wayne; DEBENEDETTO, Mikkel V.; DEGNAN, Andrew P.; DELUCCA, George V.; DESKUS, Jeffrey A.; HAN, Wen-Ching; KUMI, Godwin Kwame; SCHMITZ, William D.; STARRETT, John E., JR.; HILL, Matthew D.; HUANG, Hong; (563 pag.)WO2016/183118; (2016); 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. 27808-16-8, name is 4-Methyl-1H-1,2,3-triazole, A new synthetic method of this compound is introduced below., Formula: C3H5N3

Into a macrowave tube, 4-methyl-1 H-1 ,2,3-triazole (473 mg, 5.69 mmol) was dissolved in THF (10 ml) and cooled to 0C, NaH (341 mg, 8.54 mmol) was added and stirred for 1 h at rt. A solution of 4-(4-methoxyphenyl)butyl methanesulfonate (490 mg, 1.897 mmol) in DMF (2.00 ml) and THF (1.0 ml) was then added and heated to 60C for 3h. The mixture was diluted with EA (20 ml) and filtered through a pad of celite. The filtrate was concentrated to dryness. The crude was purified using ISCO column (DCM to 40% EA in DCM) to give two isomers. The title compound (0.13 g), 1H NMR (400 MHz, CDCb) delta ppm 1.57 – 1.64 (m, 2 H) 1.88 – 2.02 (m, 2 H) 2.29 (s, 2 H) 2.57 (t, J=7.63 Hz, 2 H) 3.78 (s, 3 H) 4.35 (t, J=7.04 Hz, 2 H) 6.76 – 6.86 (m, 2 H) 7.06 (m, J=8.22 Hz, 2 H) 7.31 (s, 1 H) and 2-(4-(4-methoxyphenyl)butyl)-4-methyl-2H-1 ,2,3-triazole (0.18 g). 1H NMR (400 MHz, CDCb) delta ppm 1.60 – 1.68 (m, 2 H) 1.80 – 1.97 (m, 2 H) 2.26 (s, 1 H) 2.33 (s, 2 H) 2.52 – 2.66 (m, 2 H) 3.78 (s, 3 H) 4.16 – 4.36 (m, 2 H) 6.82 (m, J=8.22 Hz, 2 H) 7.05 (d, J=8.61 Hz, 2 H) 7.32 (m, 1 H)

The synthetic route of 27808-16-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; UNIVERSITE DE MONTREAL; GAREAU, Yves; GINGRAS, Stephane; CHANTIGNY, Yves; YANG, Gaoqiang; SAUVAGEAU, Guy; BACCELLI, Irene; MARINIER, Anne; (284 pag.)WO2019/84662; (2019); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics