Day: December 29, 2020

Reference of 27996-86-7, 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 27996-86-7 as follows.

General procedure: To a glass vessel suitable for sealing with Teflon cap (for microwave vials) were added 1-(chloromethyl)-4,5-dimethoxy-2-nitrobenzene (1 equiv.) [34] and benzaldehyde derivative (3 equiv.) The vessel was capped and then evacuated and backfilled with N2 (thrice-repeated process). Anhydrous DMF (3.5mL/mmol) was introduced and the solution was vigorously stirred for 20minat-20C. TDAE (1.06 equiv.) was added slowly and the mixture was stirred for one hour. Then, the reaction was stirred at room temperature overnight. After LC-MS analysis clearly showed that the chloride had been totally consumed, the reaction was hydrolyzed with water. The mixture was then extracted with ethyl acetate. The combined organic layers were washed with water and brine, dried over Na2SO4, filtered off, and concentrated under reduced pressure to afford the corresponding crude product.

According to the analysis of related databases, 27996-86-7, the application of this compound in the production field has become more and more popular.

Reference:
Article; Da Costa, Laurene; Scheers, Els; Coluccia, Antonio; Rosetti, Alessia; Roche, Manon; Neyts, Johan; Terme, Thierry; Cirilli, Roberto; Mirabelli, Carmen; Silvestri, Romano; Vanelle, Patrice; European Journal of Medicinal Chemistry; vol. 140; (2017); p. 528 – 541;,
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. 6818-99-1, name is 3-Chloro-1,2,4-triazole, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 3-Chloro-1,2,4-triazole

STR18 A mixture of 34 g (246 mmol) of potassium carbonate and 35 g (338 mmol) of 3-chloro-1,2,4-triazole in 130 ml of acetone is refluxed. To this mixture there is added dropwise a solution of 50 g (169 mmol) of 2-bromo-4-chloro-1-(4-chlorophenyl)-butan-1-one in 60 ml of acetone. The mixture is boiled under reflux for a further 8 hours, the solid residue is then filtered off with suction, and the solvent is stripped off under reduced pressure. The residue which remains is taken up in ethyl acetate. The solution is washed with water, dried over sodium sulphate and concentrated under reduced pressure. The residue which remains is chromatographed on silica gel using dichloromethane as the eluent. Concentration of the elude by evaporation gives 42.9 g (90% of theory) of 1-(4-chlorobenzoyl)-1-(3-chloro-1,2,4-triazol-1-yl)-cyclopropane in the form of a solid of melting point 85 C.

According to the analysis of related databases, 6818-99-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Bayer Aktiengesellschaft; US5096913; (1992); A;,
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.

A solution of 1H-1,2,3-triazole-4-carboxylic acid (26 mg, 0.23 mmol) and HBTU (171 mg, 0.45 mmol) in a mixed solvent of dimethyl sulfoxide (2 mL) and tetrahydrofuran (4 mL) was stirred for 10 min at rt, then (+/-) -cis-6- ( (3-aminocyclohexyl) amino) -2- (5, 7-difluoro -1-tosyl-1H-indol-3-yl) -5-fluoro-4-phenylnicotinonitrile (92 mg, 0.15 mmol) and DIPEA (0.10 mL, 0.61 mmol) were added into the mixture. The resulting mixture was stirred at rt overnight. To the reaction mixture was added water (30 mL) , and the mixture was extracted with EtOAc (30 mL ¡Á 3) . The combined organic layers were washed with a saturated aqueous sodium chloride solution (60 mL) , dried over anhydrous sodium sulfate, and filtered. The filtrate was concentrated in vacuo to dry, and the residue was purified by silica gel column chromatography (PE/EtOAc (v/v) 5/1 1/5) to give the title compound as a white solid (78 mg, 73 %) . 1H NMR (400 MHz, CDCl3) delta (ppm) : 8.66 (s, 1H) , 8.20 (s, 1H) , 7.93 (d, J 8.0 Hz, 2H) , 7.71 (d, J 8.9 Hz, 1H) , 7.55 (s, 5H) , 7.31 (d, J 8.3 Hz, 2H) , 7.00 (s, 1H) , 6.84 (t, J 9.3 Hz, 1H) , 5.22 (d, J 5.7 Hz, 1H) , 4.30 (s, 1H) , 4.14 (d, J 7.2 Hz, 1H) , 2.58 (d, J 11.1 Hz, 1H) , 2.39 (s, 3H) , 2.29 (d, J 11.3 Hz, 1H) , 2.17 (d, J 11.0 Hz, 1H) , 1.97 (d, J 14.3 Hz, 1H) , 1.63 (m, 4H) .

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-4-carboxylic acid, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; SUNSHINE LAKE PHARMA CO., LTD.; TANG, Changhua; REN, Qingyun; YIN, Junjun; YI, Kai; ZHANG, Yingjun; (161 pag.)WO2018/41091; (2018); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Synthetic Route of 288-88-0, 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.

Example 91: Preparation of 4-(lH-l,2,4-triazol-l-yl)benzaldehyde (DI5) To a stirring solution of 4-fluorobenzaldehyde (10.0 g, 80.6 mmol) in DMF (150 mL) were added K2CO3 (13.3 g, 96.7 mmol) and 1,2,4- triazole (6.67 g, 96.7 mmol) and the resultant reaction mixture was stirred at 120 C for 6 h. After completion of reaction (by TLC), the reaction mixture was diluted with H20 and extracted with EtOAc (3 xlOO mL). The combined EtOAc layer was washed with H20 and brine, dried over Na2S04, and concentrated under reduced pressure to afford the title compound as a solid (9.0 g, 65%): mp 145-149 C: ]H NMR (400 MHz, CDC13) delta 10.08 (s, IH), 8.70 (s, IH), 8.16 (s, IH), 8.06 (d, J = 8.0 Hz, 2H), 7.92 (d, J = 8.0 Hz, 2H); ESIMS m/z 173.9 ([M+H]+).

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

Reference:
Patent; DOW AGROSCIENCES LLC; LO, William C.; HUNTER, James E.; WATSON, Gerald B.; PATNY, Akshay; IYER, Pravin S.; BORUWA, Joshodeep; WO2014/100163; (2014); 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. 23579-79-5, name is 3,5-Dibromo-1-methyl-1H-1,2,4-triazole, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: C3H3Br2N3

A mixture of 1,2,3, 4-tetrahydroisoquino line (1.1 g, 8.3 mmol), intermediate 32 (0.2 g, 8.3 mmol), K2C03 (2.3 g, 16.6 mmol) in DMF (20 ml) was heated at 160 C for 45 min using microwave irradiation. The r.m. was cooled and then poured onto 1?0 and extracted with DCM. The organic layer was dried (MgSC^) and concentrated under reduced pressure. The residue was purified by flash column chromatography over silica gel (eluent: DCM/MeOH from 100/0 to 97/3). The product fractions were collected and concentrated in vacuo, yielding 900 mg of intermediate 33 (40 %).

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 23579-79-5.

Reference:
Patent; ORTHO-MCNEIL-JANSSEN PHARMACEUTICALS, INC; VAN BRANDT, Sven, Franciscus, Anna; DE CLEYN, Michel, Anna, Jozef; GIJSEN, Henricus, Jacobus, Maria; BERTHELOT, Didier, Jean-Claude; SURKYN, Michel; WO2011/86099; (2011); 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. 27996-86-7, name is 4-[1,2,4]Triazol-1-yl-benzaldehyde, A new synthetic method of this compound is introduced below., category: Triazoles

General procedure: A mixture of azolyl ketone (1a/1b) (1 mmol) and aryloxy benzaldehyde (2a-f) (1 mmol) were dissolved in 10% NaOH-EtOH (5 mL), it was stirred at room temperature for 9-10 h. After completion, 5 mL water was added to the reaction mixture. The separated solid compound was filtered and washed with water. It was purified by crystallization with methanol/chloroform or basic alumina column chromatography to give the desired compounds (3-13).The compounds (16-31) were prepared by the reaction of their corresponding aldehyde and ketone partners.

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; Marrapu, Vijay K.; Chaturvedi, Vinita; Singh, Shubhra; Singh, Shyam; Sinha, Sudhir; Bhandari, Kalpana; European Journal of Medicinal Chemistry; vol. 46; 9; (2011); p. 4302 – 4310;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Related Products of 1186050-58-7, 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. 1186050-58-7, name is 2-Fluoro-6-(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.

Dissolve 2-fluoro-6- (2H- 1,2,3 -triazol-2-yl) benzoic acid (0.69 g, 3.33 mmol) with anhydrous dichloromethaneThionyl chloride (8 mL, 109.0 mmol) and DMF (0.04 mL, 0.5 mmol) were slowly added and the reaction was gradually warmed to reflux for 3 hours. The reaction was stopped, cooled and the solvent was slowly evaporated under reduced pressure. The resulting product was used directly in the next step.

The synthetic route of 2-Fluoro-6-(2H-1,2,3-triazol-2-yl)benzoic acid has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Guangdong Dongyangguang Pharmaceutical Co., Ltd.; Jin Chuanfei; Xu Juan; Zhong Wenhe; Zhang Yingjun; Liu Qi; (35 pag.)CN105949203; (2016); A;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Application of 288-36-8, These common heterocyclic compound, 288-36-8, name is 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.

EXAMPLE 1-C; 2-C2H-1.2.3-triazol-2-ylV5-methylbenzoic acid (1-5); A solution of 2-iodo-5-methylbenzoic acid (1-13, 4.0 g, 15.3 mmol) in DMF (10 mL) was treated with 1,2,3-triazole (2.1 g, 30.5 mmol), CsCO3 (9.95 g, 30.5 mmol), CuI (0.145 g, 0.76 mmol) and trans-N,N’-dimethylcyclohexane-l,2-diamine (0.43 g, 3.05 mmol). The mixture was heated at 120 0C for 10 min in a microwave reactor. The reaction was cooled to room temperature, diluted with water, and washed with EtOAc. The aqueous phase was acidified with IN HCl and extracted with EtOAc. The organic layer was dried over Na2SO4, filtered and concentrated. The residue was purified by gradient elution on SiO2 (0 to 10% MeOH in water with 0.1% AcOH) to give the faster eluting 2-(2H-l,2,3-triazol-2-yl)-5-methylbenzoic acid U5_, followed by the undesired regioisomer isomer, l-(2H-l,2,3-triazol-2-yl)-5-methylbenzoic acid (IzIA)- Data for M: 1HNMR (500 MHz, DMSO-d6) d 12.98 (br s , IH), 8.04 (s, 2H), 7.72-7.45 (m, 3H), 2.41 (s, 3H) ppm.

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

Reference:
Patent; MERCK & CO., INC.; WO2009/58238; (2009); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Reference of 41253-21-8,Some common heterocyclic compound, 41253-21-8, name is Sodium 1,2,4-triazol-1-ide, molecular formula is C2H2N3Na, 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.

3-Fluoro-2-1,2,4-triazol-1-yl-benzonitrile. A mixture of 2,3-difluorobenzylnitrile (2.27 g, 16.3 mmol) and triazole sodium salt (1.33 g, 14.8 mmol) in tetrahydrofuran (5 mL) and dimethylformamide (10 mL) was stirred at 85 C. for 4 h. After concentration, the residue was purified by flash chromatography (SiO2) eluting with 25%-50% ethyl acetate/hexane. The isolated product was recrystallized from hot ethyl acetate/hexane to give the title compound as white needles (1.51 g, 54% yield). 1H-NMR (500 MHz, CDCl3) delta ppm: 8.50 (1H, d, J=2.4 Hz), 8.25 (1H, s), 7.69-7.67 (1H, m), 7.60-7.57 (2H, m). LCMS [M+H]+ calcd for C9H6N4F: 189.16. found: 189.14.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Sodium 1,2,4-triazol-1-ide, its application will become more common.

Reference:
Patent; Bristol-Myers Squibb Company; US2007/129379; (2007); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Electric Literature 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.

[0433] 1,2,4-Triazole sodium salt (236 mg, 2.7 mmol) was added to a solution of the title compound from Example 7, Step 1 (1.9 mmol) in 1.5 ml of DMF and the resulting mixture was heated at 50 C. for 18 hours. The cooled reaction mixture was diluted with 10% aqueous sodium bicarbonate (15 ml) and extracted with three 15 ml portions of dichloromethane. The combined organic layers were dried (Na2SO4) and concentrated to an oil. Purification by flash chromatography (10 micron mesh silica gel; elution with methanol: dichloromethane, 3:97 in volume) afforded the title compound as an oil (415 mg, 70% yield). [0434] Mass spectrum: m/z 314, 316 (m, m+2). [0435] 13C NMR (125 MHz, CDCl3) delta 152.5, 143.5, 141.9, 141.6, 134.2, 133.4, 131.4, 130.3, 129.3, 127.8, 127.7, 122.6, 53.4 ppm.

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; Pfizer Inc.; US2004/229874; (2004); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics