Day: August 30, 2021

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 3112-31-0 as follows. Product Details of 3112-31-0

To a 25 mL reactor, 174.0 mg of 3,5-pyrazoledicarboxylic acid monohydrate and 250.0 mg of copper sulfate pentahydrate powder were added, 5 mL of pyridine and 10 mL of water were added, and after stirring for 15 minutes, the reaction kettle was placed in an oven and heated to 180. °C, reaction for 24 hours; After the reaction is completed, the reaction solution is transferred to a flask, and 2 mL of a saturated aqueous solution of sodium sulfide is added to the reaction solution, and after the precipitation is completed, it is filtered:Add 1M hydrochloric acid solution to the filtrate droplet obtained in the second step, adjust the solution pH=3, and filter;The filtrate obtained in the third step was extracted with an organic solvent dichloromethane (3×20 mL), and the organic phase was collected and dried over anhydrous sodium sulfate for 10 h;The organic phase obtained after the fourth step of drying was concentrated and dried to obtain 100 mg of a white powder, which was designated as sample 1.

According to the analysis of related databases, 3112-31-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Chinese Academy Of Sciences Fujian Structure Of Matter Institute; Huang Deguang; Xiang Shiqun; Zhang Xiaofeng; (13 pag.)CN109369617; (2019); A;,
Pyrazole – Wikipedia,
Pyrazoles – 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 26621-44-3 as follows. name: 3-Nitro-1H-pyrazole

3-Nitropyrazole (11.3 g, 0.1 mol) at room temperature,Benzyl bromide (17.1 g, 0.1 mol), tetrabutylammonium bromide (1.6 g, 0.005 mol), dissolved in 10 ml of dimethyl sulfoxide (DMSO).Add sodium hydroxide solution [sodium hydroxide solution: 8.8 g (0.22 mol)The solution obtained by dissolving sodium hydroxide in 10 ml of water], the reaction is exothermic,After the dropwise addition is completed, the mixture is stirred at room temperature overnight, and diluted with water to quench.Extract with dichloromethane, dry, concentrate and recrystallize with semi-dry petroleum ether.The product was obtained in 18.3 g with a yield of 90%.

According to the analysis of related databases, 26621-44-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Changsha Luxing Biological Technology Co., Ltd.; Tan Yongjun; (16 pag.)CN108863936; (2018); A;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

852227-86-2, name is 5-(Chloromethyl)-1,3-dimethyl-1H-pyrazole, belongs to pyrazoles-derivatives compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. COA of Formula: C6H9ClN2

A mixture of N-(1 -methylcyclopropyl)-3-[(1 -metriylpyrazol-4-yl)metriyl]-2-oxo- 7H-quinoline-6-sulfonamide (60 mg, 0.16 mmol), 5-(chloromethyl)-1 ,3-dimethyl- 1H -pyrazole (23 mg, 0.16 mmol), potassium carbonate (45 mg, 0.32 mmol) and potassium iodide (27 mg, 0.16 mmol) in DMF (2 mL) was heated with agitation in the microwave at deltaOmicron ‘ for 30 minutes. The solvent was removed in vacuo and the residue purified by prep HPLC (high pH) affording the desired product (20 mg, 0.042 mmol, 26%) as a white powder.

The synthetic route of 852227-86-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; CANCER RESEARCH TECHNOLOGY LIMITED; MCGONAGLE, Alison E.; JORDAN, Allan; WASZKOWYCZ, Bohdan; HUTTON, Colin; WADDELL, Ian; HITCHIN, James R.; SMITH, Kate Mary; HAMILTON, Niall M.; (497 pag.)WO2016/92326; (2016); A1;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 89607-15-8, name is 3-Bromo-1-methyl-4-nitro-1H-pyrazole, belongs to pyrazoles-derivatives 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 89607-15-8, Product Details of 89607-15-8

Step 5: Into a 100 mL round bottom flask containing a solution of 3-bromo-1-methyl-4-nitro- 1H-pyrazole (1.0 g) in ethyl acetate (50 mL) at room temperature was added Raney Nickel (700 mg) and the reaction mixture was stirred at room temperature for 16 h under hydrogen atmosphere. The reaction mixture was filtered through celite and washed with ethyl acetate. The filtrate was concentrated under reduced pressure and purified by flash chromatography eluting with ethyl acetate in petroleum ether (40-50%) to afford 3-bromo-1-methyl-1H-pyrazol-4-amine as a liquid. 1H NMR (CD3OD, 400 MHz): delta 7.18 (s, 1H), 3.77 (s, 3H). MS calc?d [M+H]+ 176.0, found 176.2

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; MERCK SHARP & DOHME CORP.; LIM, Jongwon; ALTMAN, Michael, D.; BRUBAKER, Jason, D.; GIBEAU, Craig, R.; (94 pag.)WO2016/144847; (2016); A1;,
Pyrazole – Wikipedia,
Pyrazoles – 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. 3920-40-9, name is 4-Amino-1-methyl-1H-pyrazole-3-carboxamide, A new synthetic method of this compound is introduced below., COA of Formula: C5H8N4O

Stage c A mixture of 2-(3-methanesulphonylphenyl)thiazole-4-carboxylic acid (120 mg) from stage b and 4-amino-1-methyl-1H-pyrazole-3-carboxamide (65 mg) in triethylamine (176 muL) and DMF (3 ml) in the presence of HATU (209 mg) is stirred at room temperature for 88 h. Water is added, the mixture is extracted with ethyl acetate and the organic phase is concentrated. Purification by preparative HPLC and purification by column chromatography on silica gel (mobile phase cyclohexane/acetone) result in 2-(3-methanesulphonylphenyl)thiazole-4-(3-carbamoyl-1-methyl-1H-pyrazol-4-yl)carboxamide (3.4 mg) as a white solid. C16H15N5O4S2, M=405.1; LC-MS (ZQ): Rt=0.92, m/z=406 [M+H]+. 1H-NMR (300 MHz, D6-DMSO): 3.31 (s, 3H), 3.90 (s, 3H), 7.56 (s, 1H), 7.72 (s, 1H), 7.84 (m, 1H), 8.07 (m, 1H), 8.32-8.38 (m, 2H), 8.43 (m, 1H), 8.55 (s, 1H), 11.3 (s, 1H)

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; Ulrich, BOTHE; Arne, Von Bonin; Duy, Nguyen; Ulf, Bomer; Judith, Guenther; US2009/163486; (2009); A1;,
Pyrazole – Wikipedia,
Pyrazoles – 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. 154471-65-5, name is 1-Methyl-3-(trifluoromethyl)-1H-pyrazole belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below. COA of Formula: C5H5F3N2

To a mixture of 8.71 g of l-methyl-3-trifIuoromethyl-1H-‘ pyrazole and 130 ml of tetrahydrofuran was added dropwise 32 ml of a 2.0 mol/L lithium diisopropylamide solution in heptane/tetrahydrofuran/ethylbenzene at -78C. The mixture of stirred at -780C for 2 hours and then poured into a mixture was dry ice and 50 ml of tetrahydrofuran. The mixture was stirred for 2 hours while allowing it to rise to around room temperature. Water and diethyl ether were poured into the reaction mixture. The aqueous layer was adjusted to pH 10-12 by an addition of a 2N aqueous sodium hydroxide solution, and then layers were separated. The resulting aqueous layer was washed with diethyl ether two times, adjusted to around pH 3 by an addition of 2N hydrochloric acid, and then extracted with methyl tert-butyl ether three times. The organic layers were combined, washed with an aqueous saturated sodium chloride solution, dried over magnesium sulfate, and concentrated under reduced pressure to obtain 8.19 g of l-methyl-3- tri f luoromethyl- lH-pyra zole- 5-carboxylic acid of the formula :l-Methyl-3-trifluoromethyl-lH-pyrazole-S-carboxylic acid EPO 1H-NMR (CDCl3, TMS) delta (ppm) : 4.13 (3H, s) , 7.22 (IH, s).

The synthetic route of 154471-65-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SUMITOMO CHEMICAL COMPANY, LIMITED; WO2007/43677; (2007); A1;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

Related Products of 67-51-6, These common heterocyclic compound, 67-51-6, name is 3,5-Dimethyl-1H-pyrazole, 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.

General procedure: To an 8 mL dram vial was added iodobenzene diacetate (0.6 mmol, 1.5 equiv), and heteroarene(0.4 mmol, 1 eq.), anhydrous dichloroethane (1 mL), then chloride source (5 equiv). The solutionwas allowed to stir (1000 rpm) at 50 C for the indicated amount of time. After which the solutionwas washed with saturated sodium bicarbonate, followed by saturated sodium thiosulfate andconcentrated. The crude mixture was then purified by column chromatography.

Statistics shows that 3,5-Dimethyl-1H-pyrazole is playing an increasingly important role. we look forward to future research findings about 67-51-6.

Reference:
Article; Fosu, Stacy C.; Hambira, Chido M.; Chen, Andrew D.; Fuchs, James R.; Nagib, David A.; Chem; vol. 5; 2; (2019); p. 417 – 428;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

Reference of 5203-77-0, These common heterocyclic compound, 5203-77-0, name is 1,3-Dimethyl-1H-pyrazol-5-ol, 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.

Weigh 4.0g (0.036mol) 1,3- dimethyl-5-pyrazolone-ol in 250mLthree-necked flask was added 50mL1,2-Dichloroethane was dissolved, weighing 12g (0.12mol) oftriethylamine in the system. Under ice cooling, the mixture of intermediate(b-2)The reaction solution (0.030mol press note) was addeddropwise to the system, a solution process using argon. After the reaction 1hHPLC trace transShall, after completion of the reaction raw reaction solutioncontaining the intermediate (b-3) a. To the reaction solution containingintermediate (b-3) in additional3.0g (0.030mol) of triethylamine and 0.5mL acetonecyanohydrin, temperature control and the use of argon, the reaction 2h at 50 ~60 ,The reaction was followed by HPLC. After completion of thereaction was added 100mL of water was slowly added dropwise HCl, stirring atroom temperature, until pH = 3 or so. ExtractionThe aqueous layer was removed, and the organic layer waswashed twice with 200mL of water, dried over anhydrous sodium sulfate, theorganic solvent was removed by rotary evaporation to afford 8.1gA tan solid, a powdered compound b.

The synthetic route of 5203-77-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Lian, Lei; Zheng, Yurong; He, Bin; Pengxue, Gang; Jin, Tao; Cui, Qi; (63 pag.)CN105503728; (2016); A;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 6994-25-8, name is Ethyl 3-amino-1H-pyrazole-4-carboxylate, belongs to pyrazoles-derivatives 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 6994-25-8, SDS of cas: 6994-25-8

Example 29[00239] Example 29 presents the preparation of Cmpd 29, N-(5-fluoropyrimidin-2-yl)- 4,5,6,7-tetrahydropyrazolo[3′,4′:6,7]cyclohepta[1,2-d][1 ,3]thiazol-2-amine (Table II, Compound No. 29)[00240] To a solution of t-BuONO (124 g, 1.20 mol) in 3 L MeCN was added CuBr2 (279 g, 1.20 mol). The mixture was stirred at room temperature for 1 h under nitrogen, then compound 29a (160g, 1.03 mol) was added in portions over 30 min. The mixture was stirred at room temperature under nitrogen for 30 min, then heated to 70C and stirred for an additional 2h. After cooling to r.t., the solvent was removed in vacuo. The residue was diluted with EtOAc (3 L) and washed with brine (400 mL.x3). The organic layer was dried over MgS04, filtered, and concentrated to afford the crude product 29b (200 g, 89% yield) used directly in the next step without purification.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; MERCK SHARP & DOHME CORP.; ADDEX PHARMA S.A.; LIVERTON, Nigel, J.; BOLEA, Christelle; CELANIRE, Sylvain; YUNFU, Luo; WO2012/8999; (2012); A2;,
Pyrazole – Wikipedia,
Pyrazoles – 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. 31230-17-8, name is 5-Methyl-1H-pyrazol-3-amine, This compound has unique chemical properties. The synthetic route is as follows., Product Details of 31230-17-8

The purchased 3-amino-5-methylpyrazole (20 g, 206 mmol) was dissolved in 200 ml of water and sodium bicarbonate (52 g, 618 mmol) was slowly added.Acetic anhydride (39 mL, 412 mmol) was added slowly and the system was heated to reflux overnight.After cooling, the crystals are precipitated, filtered, and washed with solid water and dried.Product A (12.4 g, 88 mmol, 43% yield) was obtained.

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 31230-17-8.

Reference:
Patent; East China Normal University; Chinese Academy Of Sciences Shanghai Pharmaceutical Institute; Lv Wei; Zhang Qiumeng; Xiao Donghuai; Shen Qianqian; Su Yi; Chen Yi; Ding Jian; (41 pag.)CN109020980; (2018); A;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics