Category: Triazoles

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 61-82-5 as follows. name: 1H-1,2,4-Triazol-5-amine

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

According to the analysis of related databases, 61-82-5, the application of this compound in the production field has become more and more popular.

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

Synthetic Route of 184177-83-1, These common heterocyclic compound, 184177-83-1, name is 1-((2S,3S)-2-(Benzyloxy)pentan-3-yl)-4-(4-(4-(4-hydroxyphenyl)piperazin-1-yl)phenyl)-1H-1,2,4-triazol-5(4H)-one, 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.

2-[(l S2S)-l-Ethyl-2-benzyloxypropyl]-2,4-dihydro-4-[4-[4-(4-hydroxyphenyl)-l- piperozinyl] phenyl]-3H-l,2,4-triazol-3-one (1 kg) was added to the Flask along with Dimethylsulfoxide (8 lit) at room temperature and stirred for 15 min. Solution of Sodium hydroxide (0.15 kg) in Water (0.3 lit) was added at same temperature and maintained for 1 hr. ((3S,5R)-5-((lH-l,2,4-triazol-l-yl)methyl)-5-(2,4- difluorophenyl)-tetrahydrofuran-3-yl)methyl-4-methylbenzene sulfonate (1.2 kg) was added and maintained for 4-5 hrs. Water (10 lit) was added to the reaction mixture and stirred for 15 min. Ethyl acetate (7.5 lit) was added and stirred for 15 min. Aqueous layer and Ethyl acetate layer were separated and aqueous layer was extracted with Ethyl acetate (3 lit). Aqueous layer and Ethyl acetate layer were separated and total aqueous layer was washed with Water (5 lit) and stirred for 15 min. Aqueous layer and Ethyl acetate layer were separated and Ethyl acetate layer was washed with brine solution. Aqueous layer and Ethyl acetate layer were separated and Ethyl acetate layer was dried over Sodium sulfate and distilled under vacuum at below 50C. The resultant crude was treated with Isopropyl alcohol (10 lit) and heated to 75-80C, maintained for material dissolved and treated with activated Carbon (0.05 kg) and maintained for 1 hr. The material was filtered through the Hyflow bed and washed with Isopropyl alcohol (1 lit). The resultant mass was cooled to room temperature, maintained for 2 hrs, filtered the solid and washed with Isopropyl alcohol (1 lit). Yield: 1.3Kg; HPLC: 98.6%.

The synthetic route of 184177-83-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; METROCHEM API PVT LTD.; NANDEPU, Venkateswara Rao; BIJJULA, Venkata krishna Reddy; BATHINA, Satyanarayana; (44 pag.)WO2019/77627; (2019); 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. 288-88-0, name is 1H-1,2,4-Triazole, A new synthetic method of this compound is introduced below., Product Details of 288-88-0

First, 3.8 g of 1,2,4-triazole were dissolved in 8 ml of NMP at 2O0C. Then,2.2 g of NaOH and 22 ml of NMP were added in portions over 1 hour, maintaining the temperature at less than 350C. The solution was stirred for 2 hours at 20C, and 7.8 g of Na2SO4 were then added. After filtration of the solid, the resulting solution was transferred to a dropping funnel, and added over 75 minutes to a solution of 14 g of crude l,3-benzenediacetonitrile-5-(bromomethyl)-alpha,alpha,alpha’,alpha’ tetramethyl (having a purity of 81.8%, containing: 3,5-bis(2-cyanoisopropyl)toluene 4.0%, l,l-dibromo-3,5-bis(2- cyanoisopropyl)toluene 10.7%, and other impurities 3.5% ) in 20 ml of NMP, cooled to -3O0C. At the end of the addition, the suspension was stirred at -300C for 18 hours, and monitored via HPLC. When the concentration of starting material is less than 0.5 percent, an amount of acetic acid sufficient to give a pH of about 6.5 to about 7.0 is added (an HPLC analysis of the crude reaction mixture showed: residual starting material 0.4%, Anastrozole 68.9%, Isoanastrozole 5.5%, 3,5-bis (2-cyanoisopropyl)toluene 7.5%, 1,1-dibromomethyl- 3,5-bis(2-cyanoisopropyl)benzene, and 15.4%, and other impurities 2.3%.). The mixture is then allowed to warm slowly to 200C, filtered, and 37 ml of toluene, 75 ml of heptane, and 37 ml of water are added. The biphasic system is stirred vigorously for 30 minutes, and the organic layer is then separated. Water, toluene, and heptane in amounts of 25 ml, 25 ml, and 50 ml, respectively, are added to the aqueous phase, and the system is stirred for 30 minutes before the organic phase is separated. Then, 10 ml of toluene and 20 ml of heptane are added to the aqueous phase, and the system is stirred for 30 minutes before the organic phase is separated. Toluene and water, 99 ml and 400 ml, respectively, are added to the aqueous phase, and the resulting biphasic system is stirred for 1 hour. The organic layer is separated and washed 3 times with a mixture of MeOH and water (3 ml and 21 ml, respectively). The final organic phase is concentrated to 45 ml under reduced pressure at 400C, and 45 ml of heptane are added dropwise over 1 hour. The resulting suspension is cooled to 00C, stirred for 1 hour, and filtered. The crude solid is dissolved in toluene (40 ml) at 4O0C, and heptane (40 ml) is slowly added under stirring. The suspension is cooled to 00C, stirred for 1 hour, EPO and filtered. The solid is driejd at 55C under reduced pressure until constant weight is achieved, yielding 5.8 g of product with a purity as follows: Anastrozole 98.45%, Isoanastrozole 0.09%, 3,5-bis (2-cyanoisopropyl)toluene 0.06%, l-bromo-3,5-bis (2- cyanoisopropyl)toluene 0.11%, l,l-dibromo-3,5-bis(2-cyanoisopropyl)toluene 0.07%, other impurities 1.22% are by HPLC.

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; SICOR, INC.; WO2006/108155; (2006); A2;,
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. 16681-70-2, name is 1H-[1,2,3]Triazole-4-carboxylic acid, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 16681-70-2

[0875] lH-1,2,3-triazole-5-carboxylic acid (3.1 mg, 27f.tmol) was combined with HATU (1 0.4 mg, 27 flillOI) in DMF(0.5 mL), and stirred for 10 minutes. DIPEA (4.8 f.LL, 27Mmol) was added and the resulting mixture was stirred for 1minute. Compound 2 (12 mg, 27 f.tmol) dissolved in DMF (1mL) was combined with added DIPEA (14.4 f.LL, 82 flillOI)followed by addition of the activated acid solution. The resultingmixture was stirred for 30 minutes then purified by reversephase chromatography (0-100% EtOAc/hexanes to yieldCompound 3 (1 0 mg).

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 16681-70-2.

Reference:
Patent; THERAVANCE BIOPHARMA R&D IP, LLC; Fleury, Melissa; Beausoliel, Anne-Marie; Hughes, Adam D.; Long, Daniel D.; Wilton, Donna A.A.; US2015/210690; (2015); 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.

in a 2000 L finished synthesis kettle, 138 kg of sodium triazole sodium salt was dissolved in 15 kg of formamide. Adding N,N-dimethylformamide mother liquor, slowly raising the temperature to 80 C at a rate of 55 C / h, and reacting at 80 C for 8 hours, Then, N,N-dimethylformamide was recovered under a vacuum of -0.085 MPa for 2.7 hours. After the completion of the collection, the mixture is transferred to a high-vacuum distillation still for fractional distillation, and the mixture is fractionated under a vacuum of 1.33 kPa and a temperature of 227 C for 8 hours, and cooled to room temperature to obtain a fluorosilazole; wherein, the formula of the specific alkylation reaction is as follows: Formula (3).

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; Shanxi Hengrun Chemical Co., Ltd.; Fan Ming; Li Cangzhen; Chen Dunguo; Chao Liumin; Wang Jianqiao; Yin Weixin; (7 pag.)CN108864165; (2018); A;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Synthetic Route of 1533519-84-4, The chemical industry reduces the impact on the environment during synthesis 1533519-84-4, name is 4-(4-Cyclopropylnaphthalen-1-yl)-1H-1,2,4-triazole-5(4H)-thione, I believe this compound will play a more active role in future production and life.

Ethanol 535g was first added to a 1L four-necked flask at room temperature.Compound IV (106.9 g, 0.4 mol) was added with stirring and compound Vb (66.9 g, 0.22 mol) was added.Slowly warm up to 50-55C under nitrogen protection. The solid dissolves completely.Potassium bicarbonate 48 g was added in portions over 60-80 minutes. After the addition, the reaction is incubated at 50-55C for 2-3 hours.The disappearance of the TLC monitoring point indicates the end of the reaction.After the reaction was completed, insoluble material was removed by hot filtration, and the resulting filtrate was slowly cooled to -5C.A large number of white solids precipitated, and 100 ml of deionized water was added dropwise to the reaction flask over 1-2 hours to crystallize sufficiently.And remove inorganic salts. After deionized water is added, it is crystallized at -5C for 2 hours and filtered.The filter cake was washed with 100 ml of 95% ice-cold ethanol. The resulting compound (IIIa) was vacuum-dried,Dry at a temperature of 50-55C for 24 hours. 127.2 g of compound (IIIa) was obtained in a yield of 94%.

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, 4-(4-Cyclopropylnaphthalen-1-yl)-1H-1,2,4-triazole-5(4H)-thione, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Zhejiang Xin Donggang Pharmaceutical Co., Ltd.; Yan Jianbo; Ma Liangxiu; Lin Yi; Hong Huabin; (16 pag.)CN107739344; (2018); A;,
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. 956317-36-5, name is 5-Methyl-2-(2H-1,2,3-triazol-2-yl)benzoic acid, This compound has unique chemical properties. The synthetic route is as follows., category: Triazoles

Ar2-COOH (1.leq) and HBTU (1.1 eq) dissolved in dichloromethane (20m1/mmol) were stirred at 25C for 0.5-2hours, then intermediates 12-17 (leq.) and DIPEA (2 eq.) dissolved in dichloromethane were added. After 18 hours the mixture was poured in an aqueous saturated solution of NaHCO3 and extracted with dichloromethane. The crude was purified by silica gel column chromatography(DCM to DCM/MeOH = 9/1)

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 956317-36-5.

Reference:
Patent; ROTTAPHARM S.P.A.; STASI, Luigi Piero; ROVATI, Lucio; ARTUSI, Roberto; BOVINO, Clara; COLACE, Fabrizio; MANDELLI, Stefano; WO2013/127913; (2013); 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. 1001401-62-2, name is 2-(2H-1,2,3-Triazol-2-yl)benzoic acid, A new synthetic method of this compound is introduced below., name: 2-(2H-1,2,3-Triazol-2-yl)benzoic acid

A mixture of 2-(2H-1,2,3-triazol-2-yl)benzoic acid (50 mg, 0.26 mmol) in thionyl chloride (2 mL) was stirred at 80C for 1 h, cooled to RT and concentrated in vacuo. The residue was dissolved in DCM (10 mL) and added to a solution of the product from step 5 (66 mg, 0.26 mmol) in DCM (1 mL) and DIPEA (0.1 ml) at 0C. The resulting mixture was stirred at RT for 12 h, poured into water and extracted with EtOAc (50 mL x 3). The combined organic layers were washed with brine, dried over MgSO4, filtered and concentrated in vacuo. The crude product was purified by Prep-TLC (50% EtOAc in petroleum ether) to give the title compound as a white solid.

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; MERCK SHARP & DOHME CORP.; LIVERTON, Nigel; BESHORE, Douglas C.; KUDUK, Scott D.; LUO, Yunfu; MENG, Na; YU, Tingting; WO2015/18027; (2015); 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. 16681-70-2, name is 1H-[1,2,3]Triazole-4-carboxylic acid, A new synthetic method of this compound is introduced below., SDS of cas: 16681-70-2

K. (2S,4R)-5-Biphenyl-4-yl-2-hydroxymethyl-2-methyl-4-[(3H-[1,2,3]triazole-4-carbonyl)-amino]-pentanoic acid propyl ester (R4=H; R7=-(CH2)2CH3) (2S,4R)-4-Amino-5-biphenyl-4-yl-2-hydroxymethyl-2-methyl-pentanoic acid (76 mg, 242 mumol) in MeCN (0.4 mL, 8 mmol) and 4 M HCl in 1,4-dioxane (242 muL, 969 mumol) was combined with propan-1-ol (0.5 mL) at 60 C. The resulting mixture was stirred until solid precipitation was observed (~30 minutes). The solvent was evaporated under vacuum and the solids were azeotroped in toluene and dried under vacuum. 1,2,3-Triazole-4-carboxylic acid (0.0274 g, 0.242 mmol), DIPEA (169 muL, 969 mumol) and HATU (92 mg, 242 mumol) were combined in DMF (0.2 mL) and stirred for 5 minutes at room temperature. This was then combined with the dried solids, predissolved in DMF (0.2 mL) and DIPEA (0.5 eq.). The resulting mixture was stirred for 15 minutes and the reaction was quenched with AcOH. The product was purified by preparative HPLC and lyophilized to yield the title compound (24 mg; purity 95%). MS m/z [M+H]+ calc’d for C25H30N4O4, 451.23. found 451.4.

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; THERAVANCE, INC.; US2012/213806; (2012); 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. 7411-23-6, name is 3,5-Dibromo-1H-1,2,4-triazole, A new synthetic method of this compound is introduced below., Quality Control of 3,5-Dibromo-1H-1,2,4-triazole

General procedure: 3,5-Dibromo-1,2,4-triazole (1; 658 mg, 2.9 mmol) or 3-chloro-1,2,4-triazole (300 mg, 2.9 mmol), o-quinone methide precursor 2 (2.9mmol), and K2CO3 (1.2 g, 8.7 mmol) were refluxed for 4 h in DMF (10mL). After completion of the reaction, the mixture was cooled, andpoured into H2O (30 mL). The precipitate formed was collected by filtration,washed with H2O, dried, and recrystallized.

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; Osipov, Dmitry V.; Osyanin, Vitaly A.; Voskressensky, Leonid G.; Klimochkin, Yuri N.; Synthesis; vol. 49; 10; (2017); p. 2286 – 2296;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics