Day: November 6, 2020

176969-34-9, 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 176969-34-9 as follows.

To a solution of 600 mg of 3-difluoromethyl-1-methyl-1H-pyrazole-4-carboxylic acid [compound (III)] and a catalytic amount of N,N-dimethylformamide in dichloromethane (7 mL), 450 mg of thionyl chloride were added dropwise. The mixture was refluxed for 2 h. The reaction was monitored by GC/MS. The solvent was evaporated in vacuo. The crude acid chloride obtained was used in the following step.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 176969-34-9, and friends who are interested can also refer to it.

1453-58-3, Adding a certain compound to certain chemical reactions, such as: 1453-58-3, name is 3-Methylpyrazole, 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 1453-58-3.

Step 1 1-(4-Methoxy-phenyl)-3-methyl-1H-pyrazole: The title compound was prepared from 4-methoxyphenylboronic acid (1.85 g, 12.1 mmol), 3-methyl-1H-pyrazoles (0.5 g, 6.1 mmol) using the general procedure A with a yield of 30% (0.4 g); MS (APCI) m/z: 189 (M+1, 100).

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, 3-Methylpyrazole, other downstream synthetic routes, hurry up and to see.

27258-33-9, Name is 1-Methyl-1H-pyrazole-5-carbaldehyde, 27258-33-9, 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.

A mixture of 1-methyl-1H-pyrazole-5-carbaldehyde (5.0 g, 45.4 mmol), N-iodosuccinimide(15.3 g, 68.1 mmol), and TFA (50 mL) was stirred at room temperature for 1.5 h. H20 (50mL) was added, and the precipitate was filtered, rinsed with H20 (100 mL), and dried toafford the title compound (9.03 g, 84%).?H NMR (500 MHz, CDC13) oe ppm 4.19 (s, 3H), 7.58 (s, 1H), 9.80 (s, 1H)

Statistics shows that 1-Methyl-1H-pyrazole-5-carbaldehyde is playing an increasingly important role. we look forward to future research findings about 27258-33-9.

These common heterocyclic compound, 25016-11-9, name is 1-Methyl-1H-pyrazole-4-carbaldehyde, 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. 25016-11-9

General procedure: To a solution of S2 (50 mg, 0.2 mmol) in 1,2-dichloroethane (DCE, 1 mL) was added aldehyde(1.1 equiv), sodium triacetoxyborohydride (79 mg, 0.5 mmol) and AcOH (25 muL, 0.5 mmol) at roomtemperature. The solution was stirred for 16 h and concentrated. The solution was extracted withethyl acetate (3 mL), washed with citric acid solution, saturated NaHCO3, and concentrated. Theremaining residue was dissolved in THF and chloroacetyl chloride (23.8 muL, 0.3 mmol) was thenadded at 0 C. The solution was warmed to room temperature and stirred for 2 h. The solutionwas concentrated and separated by preparative TLC to afford RS004 analogues.

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 25016-11-9.

35277-02-2, A common heterocyclic compound, 35277-02-2, name is 4-Fluoro-1H-pyrazole, molecular formula is C3H3FN2, 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 dry, nitrogen-purged 100 mL round-bottom flask equipped with a dropping funnel under argon atmosphere, NaH of 60% dispersion in mineral oil (674 mg, 16.9 mmol) was added in 60 mL of anhydrous THF solvent in the flask at ice-water bath, and 4-fluoro-1H-pyrazole (691 mg, 8.03 mmol) was stirred in over 30 min at the ice-water bath. Into the flask, the solution of (R)-3-bromo-2- hydroxy-2-methyl-N-(4-nitro-3-(trifluoromethyl)phenyl)propanamide (2.98 g, 8.03 mmol) in 10 mL of anhydrous THF was added through dropping funnel under argon atmosphere at the ice-water bath and stirred overnight at room temperature. After adding 1 mL of H2O, the reaction mixture was condensed under reduced pressure, and then dispersed into 50 mL of EtOAc, washed with 50 mL (x 2) water, evaporated, dried over anhydrous MgSO4, and evaporated to dryness. The mixture was purified with flash column chromatography as an eluent EtOAc/hexane = 1/2 to produce designed compound (2.01 g, 67%) as yellowish solid.MS (ESI) m/z 375.08 [M- H]-; 377.22 [M + H] +; 399.04 [M + Na]+;19F NMR (CDCl3, decoupled) d -60.13, -176.47; assigned by NOE and COSY; 1H NMR (400 MHz, CDCl3) d 9.14 (bs, 1H, NH), 8.01 (s, 1H), 7.97-7.91 (m, 2H), 7.38 (d, J = 3.6 Hz, 1H), 7.35 (d, J = 4.4 Hz, 1H), 5.95 (s, 1H, OH), 4.56 (d, J = 14.0 Hz, 1H), 4.17 (d, J = 14.0 Hz, 1H), 1.48 (s, 3H).

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

5334-40-7, 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. 5334-40-7, name is 4-Nitro-1H-pyrazole-3-carboxylic acid, This compound has unique chemical properties. The synthetic route is as follows.

N-Benzylthanolamine (2.147 mL, 1.06 g/mL, 15.052 mmol) and 4-nitro-1H-pyrazole-3- carboxylic acid (2 g, 12.732 mmol) in toluene (13.8 14 mL) were stirred at 15¡ãC. SOC12 (2.554 mL, 1.64 g/mL, 35.206 mmol) was slowly added followed by DMF (96.907 jiL,0.944 g/mL, 1.252 mmol). The reaction mixture was stirred at 55¡ãC for 10 minutes then70¡ãC for 1 8h. The reaction was allowed to cool to room temperature and then the solvents were evaporated in vacuo. The residue was taken up into DMF (11.655 mL) and triethylamine (9.4 15 mL, 0.728 g/mL, 67.732 mmol) was added slowly. The reaction mixture was stirred at rt for 1 2h. Water was added. The mixture was extracted twice withEtOAc, dried over MgSO4, filtered and concentrated in vacuo to give 4.4g of crude material. A purification was performed via preparative LC (Stationary phase: irregular SiOH 15-40jim 120g Grace, Mobile phase: gradient from 100percent DCM to 97percent DCM, 3percent MeOH, 0.3percentNH4OH) to give 1.7g of intermediate 133b (41percent).

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.

14521-80-3, 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. 14521-80-3, name is 3-Bromo-1H-pyrazole, A new synthetic method of this compound is introduced below.

Production Example 1; (1) A mixture of 10.7 g of 3-bromo-1H-pyrazole, 11.8 g of 2,3-dichloropyridine, 57.3 g of cesium carbonate and 80 mL of N,N-dimethylformamide was stirred at 100C for 8 hours. After cooling to room temperature and adding water, the reaction mixture was extracted twice with methyl tert-butyl ether. The organic layers were combined, washed sequentially with water and a saturated sodium chloride solution, dried over magnesium sulfate, and concentrated under reduced pressure. The resulting residue was subjected to silica gel column chromatography to obtain 12.9 g of 2-(3-bromo-1H-pyrazol-1-yl)-3-chloropyridine. 2-(3-bromo-1H-pyrazol-1-yl)-3-chloropyridine 1H-NMR (CDCl3, TMS) delta (ppm): 6.51 (1H, d, J=2Hz), 7.31 (1H, dd, J=8Hz, 4hz), 7.91 (1H, dd, J=8Hz, 1Hz), 8.04 (1H, d, J=2Hz), 8.45 (1H, dd, J=4Hz, 1Hz)

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.

16617-46-2, These common heterocyclic compound, 16617-46-2, name is 3-Amino-1H-pyrazole-4-carbonitrile, 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.

– Synthesis of Intermediate Compound (4) – 4.5 parts of Compound (3) was added to 45 parts of phosphoric acid and dissolved by heating at 38¡ãC. The resulting solution was cooled on ice and kept at -3 to 0¡ãC, and 3.0 parts of sodium nitrite were added thereto and stirred for 1 hour to give a diazonium salt solution. Separately, 10 parts of Compound (2) synthesized above were dissolved in 30 parts of methanol to prepare a solution of Compound (2). The above diazonium salt solution was added thereto at 8¡ãC or less. Simultaneously with the completion of the addition, the ice bath was removed, and the mixture was stirred for 2 hours. The reaction solution was added to 300 parts of water at 10¡ãC under stirring and stirred for additional 1 hour. Precipitated crystals were separated by filtration and sufficiently washed with water. The crystals were dried to give 12.5 parts of Intermediate Compound (4). The yield was 83.4percent.

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 16617-46-2.

14521-80-3, A common heterocyclic compound, 14521-80-3, name is 3-Bromo-1H-pyrazole, molecular formula is C3H3BrN2, 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 compound 246.la (4g, 15.9mmol, 1.Oeq) and compound 1.2 (3.69g, 17.5mmol, 1.leq) in tetrahydrofuran (32mL), sodium carbonate (4.3g, 31.8mmol, 2.Oeq) was added. Reaction mixture was degassed for 5 mm. Then, [1,1?- Bis(diphenylphosphino)ferrocene]dichloropalladium(II) (1.16g, 1.59mmol, 0.leq) was added and again degassed for 5 mm. Reaction mixture was stirred at 120 C for 4h. After completion of the reaction, the reaction mixture was transferred to water and extracted with ethyl acetate. Organic layers were combined, dried over anhydrous Na2SO4, filtered and concentrated in vacuo to get the crude material. This was purified by column chromatography using 13% ethyl acetate in hexane as eluant to obtain 287.1 (2.Og, 15.49%). MS(ES): m/z 238.46 [M+H]t

The synthetic route of 14521-80-3 has been constantly updated, and we look forward to future research findings.

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 2820-37-3 as follows. 2820-37-3

To a solution of crude reactant (249.5 mg, 0.629 mmol, theoretical amount) in anhydrous THF (5 mL) was added 3.4-dimethyl-lH-pyrazole (120.7 mg, 1.256 mmol) followed by potassium carbonate (173.6 mg, 1.256 mmol). The solution was stirred at 25 C overnight then the solution was diluted with ethyl acetate (200 mL). The resulting solution was washed with brine (2x100mL), dried over magnesium sulfate and concentrated in vacuo. The crude product was purified by silica gel chromatography (petroleum ether/ ethyl acetate =1 :3) to afford product (56 mg, 0.136 mmol, Yield=22% (2 steps)) as white solid. 1HNMR (400 MHz, CDC13) 5(ppm): 7.08 (1H, s), 4.77 (1H, AB), 4.76 (1H, AB), 2.55 (1H, t), 2.18 (3H, s), 1.00-2.20 (24H, m).0.67 (3H, s). LCMS: rt = 2.41 mm, m/z = 413.2 [M+H]+

According to the analysis of related databases, 2820-37-3, the application of this compound in the production field has become more and more popular.