Day: April 19, 2021

Adding a certain compound to certain chemical reactions, such as: 2075-46-9, name is 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 2075-46-9, name: 4-Nitro-1H-pyrazole

General procedure: To a solution of compound 18 (1.1 g, 10.0 mmol) and K2CO3 (2.1 g,15.0 mmol) in MeCN (20 mL) was added iodomethane (1.6 g,11.0 mmol) at room temperature. The reaction mixture was stirredovernight at 82 C. TLC showed the completion of the reactin. The resultingmixture was removed under vacuum. Water (20 mL) was addedto the residue, and the resultant mixture was extracted with EtOAc(2 ¡Á 50 mL). The organic layers were then washed with water followed by brine. The organic layers were dried over anhydrous sodium sulfate,filtered, and concentrated to provide 19a as a yellow solid(1.2 g,9.8 mmol, 98%) without further purification. MS (ESI) m/z: 128.1 [M+H]+

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-Nitro-1H-pyrazole, and friends who are interested can also refer to it.

Reference of 35344-95-7, The chemical industry reduces the impact on the environment during synthesis 35344-95-7, name is 1H-Pyrazole-4-carbaldehyde, I believe this compound will play a more active role in future production and life.

1H-pyrazole-4-carbaldehyde (0.5 g; 5.2 mmol) and cesium carbonate (3.39 g; 10.4mmol) were diluted in ACN (10 mL). Then, 2-bromoethyl methyl ether (0.636 mL; 6.77 mmol) was added and the reaction mixture was refluxed for 2 hours. The reaction mixture was partitionned between a saturated solution of NaHCO3 and EtOAc. The organic layer was separated, dried over MgSO4, filtered and concentrated.The residue was purified by silica gel chromatography (irregular Si02, 120 g, DCM/MeOH: 100/0 to 95/5). The fractions containing the product were mixed andconcentrated to afford 439 mg (55percent) of intermediate 35.

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-Pyrazole-4-carbaldehyde, 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. 20154-03-4, name is 3-(Trifluoromethyl)-1H-pyrazole belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below. Application In Synthesis of 3-(Trifluoromethyl)-1H-pyrazole

Reference Synthesis Example 53 (0635) Ethyl 2-[3-(trifluoromethyl)-1H-pyrazol-1-yl]acetate (0636) To a chloroform solution (2 mL) of 3-(trifluoromethyl)-1H-pyrazole (68 mg, 0.50 mmol), potassium carbonate (104 mg, 0.75 mmol) and ethyl bromoacetate (100 mg, 0.60 mmol) were added and the resultant mixture was stirred at 70¡ã C. for 2 hours. To the reaction solution, adequate amount of sodium iodide was added and the resultant mixture was further stirred for 1 day. To the reaction solution, 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (147 mg, 0.77 mmol), 1-hydroxybenzotriazole (catalytic amount) and ethanol (500 muL) were added and the resultant mixture was stirred for 2 hours. After completion of the reaction, water was added to the reaction solution and extraction with chloroform from the resultant mixture was performed. The organic layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure to obtain a crude product of the title compound. The crude product was used in the next reaction as it was.

The synthetic route of 20154-03-4 has been constantly updated, and we look forward to future research findings.

Electric Literature of 37622-90-5, A common heterocyclic compound, 37622-90-5, name is Ethyl 4-pyrazolecarboxylate, molecular formula is C6H8N2O2, 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 solution of 1H-pyrazole-4-carboxylic acid ethyl ester (35.0 g, 0.25 mole) in THF (100 mL) was added suspension of sodium hydride (17.38 g, 0.43 mole) in THF (100 mL) solution under N2 at 25 C and stirred for one hour. Methyl iodide (24 mL, 0.38 mole) was added at RT and the reaction mixture was heated to 60-65 C for6 hours. Reaction mixture was quenched in to ice water (200 mL) and extracted with ethyl acetate (100 mL x 3). The combined organic phase was washed with water (50 mL), brine solution (50 mL), dried over Na2504 and concentrated under vacuum to obtain ethyl 1-methyl- 1H-pyrazole-4-carboxylate.Yield: 32.36 g (83 %); ?H – NMR (CDC13, 400 MHz) oe ppm: 1.30 – 1.33 (s, 3H), 3.91(s, 3H), 4.25 – 4.30 (q, 2H), 7.83 (s, 1H), 7.88 (s, 1H); Mass (mlz): 155.0 (M+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.

Electric Literature of 66121-71-9, These common heterocyclic compound, 66121-71-9, name is 4-Cyano-1-methylpyrazole, 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.

dissolved in Et2O (30 mL) and was added, and the the solution stirred for 30 min. 1 -Methyl- lH-pyrazole-4-carbonitrile (1 g, 9.34 mmol) was added in Et2O (20 mL) at -78 0C and the reaction was allowed to warm to room temperature over 1 h, then MeOH (10 mL) containing ammonium acetate (0.720 g, 9.34 mmol) was added. The solvents were evaporated and the residue taken up in DCM and water. The organic layer was separated and the aqueous phase extracted with DCM. The combined organic phases were shaken with Brine and dried over MgSO4, filtered and the solvent evaporated to give the product (1.4 g, 68% yield): MS (ES) m/z 220 [M+l]+.

Statistics shows that 4-Cyano-1-methylpyrazole is playing an increasingly important role. we look forward to future research findings about 66121-71-9.

Synthetic Route of 96799-02-9, 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. 96799-02-9, name is 5-(Furan-2-yl)-1H-pyrazol-3-amine, This compound has unique chemical properties. The synthetic route is as follows.

EXAMPLE 22 6-(2-Furyl)-1H-imidazo[1,2-b]pyrazole A solution of 2.0 g of 5-(2-furyl)-3-aminopyrazole in 5 ml of dimethylformamide was slowly added dropwise at room temperature, whilst stirring, to 0.59 g of a 55% w/w suspension of sodium hydride in mineral oil, which itself was suspended in 15 ml of dimethylformamide, and the resulting mixture was stirred for 1 hour at room temperature. 2.7 g of 2,2-dimethoxyethyl bromide were then added, and the mixture was allowed to react at 60 to 70 C. for 4 hours. At the end of this time, the resulting mixture was partitioned between ethyl acetate and water. The organic layer was washed with water and dried over anhydrous magnesium sulfate. The solvent was then removed by evaporation under reduced pressure. The residue was purified by silica gel column chromatography using a 1:1 by volume mixture of ethyl acetate and hexane as the eluent, to afford 1.2 g of an intermediate compound as an oil. A mixture of 1.2 g of this intermediate compound, 10 ml of a 4N solution of hydrogen chloride in dioxane and 4 ml of ethanol was heated under reflux for 20 minutes, after which the reaction mixture was poured into ice water and made basic by the addition of aqueous ammonia. The mixture was then extracted with ethyl acetate. The extract was washed with an aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate, after which the solvent was removed by evaporation under reduced pressure. The residue was purified by silica gel column chromatography using a 1:1 by volume mixture of ethyl acetate and hexane as the eluent, and the product was recrystallized from a mixture of ethyl acetate and hexane, to afford 0.44 g of the title compound as pale brown needle-like crystals, melting at 186 to 188 C. Elemental analysis: Calculated for C9 H7 N3 O: C, 62.42%; C, 4.07%; N, 24.27%. Found: C, 62.36%; H, 4.23%; N, 24.14%.

The chemical industry reduces the impact on the environment during synthesis 5-(Furan-2-yl)-1H-pyrazol-3-amine. I believe this compound will play a more active role in future production and life.

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 2075-46-9 as follows. Quality Control of 4-Nitro-1H-pyrazole

A mixture of 4-nitro-1H-pyrazole (10 g, 88 mmol) and 5% palladium on Al2O3 (1 g) in a mixture of ethanol (150 mL) and 50% aqueous HBr (50 mL) was shaken in a Par apparatus under hydrogen (10 psi) for 36 h. The mixture was filtered and the catalyst washed with ethanol. The filtrate was concentrated in vacuo to give a white solid. This solid was suspended in 10 mL of ethanol. After swirling the flask for 5 min, ether was added to complete the crystallization. The solid was filtered, was washed with ether and dried under high vacuum to afford 5-bromo-1H-pyrazol-4-amine, HBr (18.1 g, 84% yield) as a white solid: mp 248 C. dec; 1H NMR (400 MHz, DMSO-d6) delta 11.47 (s, 1H), 10.00 (s, 1H), 7.79 (s, 1H).

According to the analysis of related databases, 2075-46-9, the application of this compound in the production field has become more and more popular.

Application of 112029-98-8, These common heterocyclic compound, 112029-98-8, name is (1-Methyl-1H-pyrazol-4-yl)methanol, 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.

Under a stream of nitrogen, cyanomethylenetributylphosphorane (0.06 mL) was dropped into a 0.2-mL toluene solution of the compound (30 mg) produced in Reference Example 20, and (1-methylpyrazol-4-yl)methanol (9.6 mg), and the mixture was stirred overnight at 100C. The reaction mixture was concentrated under reduced pressure, and the resulting residue was purified by silica gel column chromatography to obtain the title compound (7 mg) having the following physical property values. 1H-NMR (CDCl3): delta 1.26, 1.39-1.42, 1.68-1.85, 2.28-2.51, 2.55-2.65, 2.83-3.05, 3.87-4.01, 4.04-4.18, 4.89, 6.40, 6.72-6.79, 7.06-7.38, 7.41, 7.51, 8.77, 9.13.

The synthetic route of 112029-98-8 has been constantly updated, and we look forward to future research findings.

These common heterocyclic compound, 1124-16-9, name is 5-Amino-1-isopropyl-3-methylpyrazole, 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. Recommanded Product: 5-Amino-1-isopropyl-3-methylpyrazole

2-[(5-Chloro-2-{[3-methyl-1-(1-methylethyl)-1H-pyrazol-5-yl]amino}-4-pyridinyl)amino]benzonitrile The solution of 2-[(2,5-dichloro-4-pyridinyl)amino]benzonitrile (110 g, 396 mmol), 3-methyl-1-(1-methylethyl)-1H-pyrazol-5-amine (55.1 g, 396 mmol), and cesium carbonate (387 g, 1187 mmol) in 1,4-dioxane (2.5 L) was degassed by N2 stream, and 2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (BINAP) (19.71 g, 31.7 mmol) followed by palladium acetate (3.55 g, 15.83 mmol) were added. The reaction mixture was heated to reflux for overnight under N2. The reaction mixture was filtered and the liquid was concentrated. Ethyl acetate (1500 mL), followed by 1 M HCl (1000 mL) were added. Layers were separated. Ethyl acetate was washed with 1 M HCl until no product was observed by HPLC (1000 mL total, 1*). HCl phases were combined, and backwashed with ethyl acetate (3*1000 mL), until the product peak was relativity pure in the HCL layer. The HCl layer was then basified with NaOH (50 w/w followed by 1 M) to ph~4 resulting in a cloudy solution. Ethyl acetate (2000 mL) was added and layers were separated. The ethyl acetate was washed with brine and evaporated. After neutralization-after addition of ethyl acetate-the reaction mixture was filtered to get some product. Also isolation of product during evaporation can be done by filtration of white solid, which comes from the mother liquor. All solids and evaporated products were combined. 2-[(5-Chloro-2-{[3-methyl-1-(1-methylethyl)-1H-pyrazol-5-yl]amino}-4-pyridinyl)amino]benzonitrile (80 g, 207 mmol, 52.4% yield) was isolated as a yellow solid. 1H NMR (400 MHz, DMSO-d6) delta ppm 1.24 (d, J=6.57 Hz, 6H) 2.08 (s, 3H) 4.34 (quin, J=6.57 Hz, 1H) 5.87 (s, 1H) 5.97 (s, 1H) 7.41 (td, J=7.58, 1.01 Hz, 1H) 7.47 (d, J=8.08 Hz, 1H) 7.75 (td, J=7.83, 1.52 Hz, 1H) 7.90 (dd, J=7.83, 1.52 Hz, 1H) 7.94 (s, 1H) 8.42 (d, J=17.43 Hz, 2H); HPLC Rt=2.36 min, MS (ESI): [M+H]+=367.1, 368.1.

The synthetic route of 5-Amino-1-isopropyl-3-methylpyrazole 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. 5334-40-7, name is 4-Nitro-1H-pyrazole-3-carboxylic acid, This compound has unique chemical properties. The synthetic route is as follows., Computed Properties of C4H3N3O4

Thionyl chloride (3.8 ml, 52.5 mmol) was added cautiously to a stirred, ice-cold mixture of 4-nitropyrazole-3-carboxylic acid (7.5 g, 47.7 mmol) in MeOH (150 ml), the mixture stirred at ambient temperature for 1 hour then heated at reflux for 3 hours. The reaction mixture was cooled, evaporated in vacuo then azeotroped with toluene to give 4-nitro-lH-pyrazole-3-carboxylic acid ethyl ester (8.8 g).

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 5334-40-7.