Category: 26621-44-3

26621-44-3, 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.

10.0 g (88.4 mmol) of 3-nitropyrazole and 14.4 g (97.2 mmol) of 2,3-dichloropyridine were initially charged in 50 ml of dimethylformamide, 23.9 g (173 mmol) of potassium carbonate were added and the reaction mixture was stirred at 125 C. for 18 hours. After cooling, the mixture was poured into water and the precipitated solid was filtered off. Recrystallization from isopropanol/water gave 18.1 g (90% of theory) of 3-chloro-2-(3-nitro-1H-pyrazol-1-yl)pyridine (log P: 1.83; MH+: 225.1; 1H-NMR (400 MHz, CD3CN, delta, ppm): 7.15 (s, 1H), 7.56 (d, 1H), 8.15 (d, 1H), 8.23 (d, 1H), 8.53 (m, 1H).

According to the analysis of related databases, 3-Nitro-1H-pyrazole, the application of this compound in the production field has become more and more popular.

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. 26621-44-3, name is 3-Nitro-1H-pyrazole, A new synthetic method of this compound is introduced below., 26621-44-3

To a solution of 3-nitro-1H-pyrazole (25 g, 221.09 mmol, 1 eq) in DMF (300 mL) was added NaH (10.61 g, 265.31 mmol, 60 wt.% in mineral oil, 1.2 eq) at 0 C under N2. The suspension was stirred at 0 C for 0.5 hour, then 2-bromopropane (27.19 g, 221.09 mmol, 1 eq) was added dropwise to the reaction mixture at 0 C. The reaction mixture was stirred at 15 C for 12 hours. The reaction mixture was quenched with saturated aqueous NH4Cl solution (200 mL), diluted with water (500 mL) and extracted with EtOAc (3 ¡Á 500 mL). The organic phases were washed with brine (500 mL), dried over anhydrous Na2SO4, filtered and concentrated in vacuum. The residue was purified by column chromotography (SiO2, Petroleum ether: Ethyl acetate, 1:0 to 5 :1) to give the title compound (15 g, 43.73% yield) as a yellow oil.1H NMR (400 MHz, CDCl3): d 7.49 (d, 1 H), 6.89 (d, 1 H), 4.65-4.54 (m, 1 H) and 1.57 (d, 6 H).

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.

Adding a certain compound to certain chemical reactions, such as: 26621-44-3, name is 3-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 26621-44-3, 26621-44-3

K2003 (48.9 g, 353.8 mmol) is added to a solution of 3-nitro-1H-pyrazole (20.0 g,176.9 mmol) in THF (200 mL) followed by 2-bromo-ethanol (18.8 mL, 265.3 mmol) and the mixture is heated under reflux for 24 h. After cooling, the mixture is partitioned between water (200 mL) and EtOAc (200 mL). The phases are separated and the aqueous phase is extracted with EtOAc (2 x 200 mL). The combined organic phases aredried (MgSO4), filtered and concentrated in vacuo. The crude residue is purified by trituration from Et20, the solid is collected by filtration and washed with Et20, DCM and Et20 again. The filtrate is concentrated in vacuo and is triturated from Et20. The solids are combined to give the title compound (18.1 g, 64 % yield) as an off-white solid.

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-Nitro-1H-pyrazole, other downstream synthetic routes, hurry up and to see.

26621-44-3, Name is 3-Nitro-1H-pyrazole, 26621-44-3, 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.

Into a 250-mL round-bottom flask was placed a solution of 3-nitro-lH-pyrazole (10 g, 88.4 mmol) in DMF (100 mL). This was followed by the addition of NaH (60% wt, 3.9 g, 97.5 mmol) in portions at 0C. The resulting solution was stirred for 0.5 h at 0C. This was followed by the addition of 2-bromopropane (14.1 g, 114.6 mmol) dropwise with stirring at 0C in 10 min. The resulting solution was stirred for 16 h at RT and then was quenched by the addition of 100 mL of water. The resulting solution was extracted with 3×100 mL of ethyl acetate. The organic layers were combined and dried over anhydrous Na2S04, then concentrated under vacuum. The residue was applied onto a silica gel column and eluted with a gradient of ethyl acetate/petroleum ether (1 :5 to 1 :3). This resulted in 11.8 g (86%) of the title compound as yellow oil. MS-ESI: 156.1 (M+l).

Statistics shows that 3-Nitro-1H-pyrazole is playing an increasingly important role. we look forward to future research findings about 26621-44-3.

26621-44-3, 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. 26621-44-3, name is 3-Nitro-1H-pyrazole belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

MC-163-1 (2 g, 17.68 mmol, 1.0 eq), p-toluenesulfonic acid (336 mg, 1.668 mmol, 0.1 eq) was dissolved in 40 mL of tetrahydrofuran.Then DHP (1.6 g, 19.448 mmol, 1.1 eq) was added. The reaction was carried out at room temperature for 16 hours.The reaction solution was added with water 25 mL, and ethyl acetate 35 mL was extracted three times.The organic phase was washed with saturated brine and dried over anhydrous sodiumPurified by column (petroleum ether: ethyl acetate 20:1 to 5:1)Get oil MC-158-1(3.5g, 99%).

The synthetic route of 3-Nitro-1H-pyrazole has been constantly updated, and we look forward to future research findings.

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. 26621-44-3, name is 3-Nitro-1H-pyrazole, This compound has unique chemical properties. The synthetic route is as follows., 26621-44-3

At room temperature, water (15 mL) was added to a mixture of 3-nitro-1H-pyrazole (48a) (1 g, 8.90 mmol) and NBS (1.73 g, 9.70 mmol), and the reaction was stirred overnight. After thin layer chromatography indicated the reaction was complete, the reaction solution was diluted with water, extracted with ethyl acetate, washed with saturated brine, dried over anhydrous sodium sulfate, concentrated under reduced pressure, and rotary evaporated to dryness, to afford compound (48b) (1.66 g, yield: 93%, white solid). MS (ESI, m/z): 192 [M+H]+.

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These common heterocyclic compound, 26621-44-3, name is 3-Nitro-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. 26621-44-3

Added to a 100mL single-necked flask 3g compound 3 and 18mL acetic acid, stirred, off-white cloudy liquid. Under cold water bath conditions 2.4mL of fuming nitric acid was slowly added dropwise to the mixed solution, maintaining vigorous stirring, turbid liquid becomes yellow, ensure that the reaction temperature does not exceed 30 deg. C. 6mL acetic anhydride was added to the mixture, after dropping, the mixture quickly became clear, dark yellow clear liquid. After the dropwise addition was stirred at room temperature for 3h. After completion of the reaction, the solution was slowly poured into 100mL crushed ice and stirred vigorously, a yellow precipitate was precipitated, filtered to give a white crystalline powder 2.0g, the filtrate was extracted with ethyl acetate to give pale yellow crystals 1.5608g. Yield: 84.7%, recrystallized from n-hexane. Weigh 50mg of compound 4 into thick-walled pressure bottle, and slowly warmed to 140 deg. C, 160 deg. C, 180 deg. C, at this temperature the reaction 1 ~ 3h to give the compound 5, the results shown in Table 2.

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 26621-44-3.

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. 26621-44-3, name is 3-Nitro-1H-pyrazole, This compound has unique chemical properties. The synthetic route is as follows., 26621-44-3

To a mixture of 3-nitro-iH-pyrazole (30 g, 265.31 mmol, 1 eq) in DMF (300 mL) was added NaH (11.14 g, 278.58 mmol, 60% purity in mineral oil, 1.05 eq) in portions at o C. Then the reaction mixture was stirred at o C for 0.5 hour. 2-Bromopropane (39.16 g, 318.37 mmol, 1.2 eq) was added and the resulting mixture was warmed to 25 C for 12 hours. The reaction mixture was quenched with water (500 mL) and extracted with EtOAc (3 x 300 mL). The combined organic layers were washed with brine (100 mL), dried over anhydrous Na2S04, filtered and concentrated in vacuo. The residue was purified by chromatography (Si02, petroleum ether: ethyl acetate, 50:1 to 2:1) to give the title compound (29.2 g, 71 %) as a yellow oil. (0810) NMR (400 MHz, CDCI3) d 749 (d, 1 H), 6.90 (d, 1 H), 4-634-56 (m, 1 H) and 1.58 (d, 6 H).

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.

A common compound: 26621-44-3, name is 3-Nitro-1H-pyrazole, belongs to pyrazoles-derivatives compound, it can change the direction of chemical reaction, and react with certain compounds to generate new functional products. A new synthetic method of this compound is introduced below. 26621-44-3

Sodium hydride (0.425 g of a 60%dispersion in mineral oil, 10.612 mmol) was added to a solution of 3-nitro-1H-pyrazole (1.000 g, 8.843 mmol) in 40 mL of THF at 0 C and the mixture was stirred for 10 min. SEM-Cl (1.72 mL, 9.727 mmol) was added dropwise and the mixture was stirred at r.t. for 1 h. The reaction mixture was diluted ethyl acetate and washed with brine. The organic phase was dried over Na2SO4, concentrated and purified by silica gel flash chromatography (EA: PE =0 to 40%) to give 1.8 g of the title compound. Yield: 86%. MS (ESI, m/e) : 244 [M+1] +.

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, 26621-44-3, other downstream synthetic routes, hurry up and to see.

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. 26621-44-3, name is 3-Nitro-1H-pyrazole belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below. 26621-44-3

General procedure: 3-methoxy-1H-pyrazole 14f (0.15 g, 1.53 mmol) was dissolved in dry pyridine (15 mL) and DMAP (0.02 g, 1.15 mmol) was added, followed by hexyl isocyanate (0.33 mL, 2.3 mmol). The resulting solution was stirred under nitrogen atmosphere at rt for 12 h. The solvent was evaporated under reduced pressure and the two regioisomers 23f and 24f were obtained in a ratio of 92:8, determined by 1H NMR of the crude. The mixture was separated by silica gel column chromatography using cyclohexane/EtOAc. 23f eluted with cyclohexane/EtOAc 99.5:0.5 and 24f eluted with cyclohexane/EtOAc 90:10.

The synthetic route of 26621-44-3 has been constantly updated, and we look forward to future research findings.