Month: April 2021

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. 39806-90-1, name is 4-Iodo-1-methyl-1H-pyrazole, A new synthetic method of this compound is introduced below., HPLC of Formula: C4H5IN2

Reference Example 140 tert-butyl ({4-(2-fluorophenyl)-5-[(1-methyl-1H-pyrazol-4-yl)thio]-1,3-thiazol-2-yl}methyl)methylcarbamate To a solution of 2-ethylhexyl 3-{[2-{[(tert-butoxycarbonyl)(methyl)amino]methyl}-4-(2-fluorophenyl)-1,3-thiazol-5-yl]thio}propanoate (356 mg) in ethanol (4 mL) was added sodium ethoxide (89 mg) at 0 C., and the mixture was stirred at room temperature for 1 hr, and concentrated under reduced pressure. A mixture of the residue, 4-iodo-1-methyl-1H-pyrazole (155 mg), tris(dibenzylideneacetone)dipalladium(0) (32 mg) and 9,9-dimethyl-4,5-bis(diphenylphosphino)xanthine (39 mg) was stirred in toluene (5 mL) at 80 C. for 2 hr. The reaction mixture was allowed to cool to room temperature, water was added, and the mixture was extracted with ethyl acetate. The extract was washed successively with saturated aqueous sodium hydrogen carbonate solution, water and saturated brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was purified by basic silica gel column chromatography (eluent: hexane-ethyl acetate=1:1) to give the title compound as a yellow oil (208 mg, yield 27%). 1H-NMR (CDCl3) delta: 1.46 (9H, brs), 2.94 (3H, brs), 3.85 (3H, s), 4.58-4.62 (2H, m), 7.15-7.26 (2H, m), 7.37-7.44 (3H, m), 7.48-7.53 (1H, m).

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.

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. 3524-32-1, name is 5-Amino-1,3-dimethylpyrazole, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 5-Amino-1,3-dimethylpyrazole

General procedure: A mixture of salicylaldehydes 1 (1 mmol), 4-hydroxy-6-methyl-2H-pyran-2-one 2 (1mmol) and L-proline (0.10 mmol) in EtOH (10 mL) was stirred at 80 C for 1 h. Then pyrazol-5-amines 3(1 mmol) and CuSO4 (0.20 mmol) was added to the reactor and stirred at 80 C for 4-48 h. Aftercompletion of the reaction confirmed by TLC (eluent acetone/petroleum ether (PE), V/V = 1:3), thereaction mixture was concentrated in vacuo to remove the solvent. The product purified by columnchromatography (PE-acetone = 5:1) to afford the pure product 4.

According to the analysis of related databases, 3524-32-1, 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. 3398-16-1, name is 4-Bromo-3,5-dimethylpyrazole, A new synthetic method of this compound is introduced below., SDS of cas: 3398-16-1

with reflux condenser and magnetic force to the rotor of the dry three-mouth bottle is sequentially added in the 3, 5 – dimethyl -4 – brompyrazole (5250 mg, 30 . 00 mmol, 1 . 00 equivalent), cuprous iodide (572 mg, 3 . 00 mmol, 0 . 10 equivalent), L – proline (690 mg, 6 . 00 mmol, 0 . 20 equivalent), potassium carbonate (8280 mg, 60 . 00 mmol, 2 . 00 equivalent) replacing nitrogen three times, then adding iodine anisole (10500 mg, 45 . 00 mmol, 1 . 50 equivalent) and steams again dimethyl sulfoxide (10 ml). The reaction mixture to the 120 C under stirring 2 days, TLC thin layer chromatographic monitoring until the raw material 4 – brompyrazole reaction finishes. The addition of water (100 ml) quenching the reaction, filtration, 50 ml ethyl acetate full washing insolubles, separating the mother liquor in the organic phase, dried with anhydrous sodium sulfate, filtered, the solvent removed by reduced pressure distillation. The obtained crude product through the silica gel column chromatography separation and purification, eluent (petroleum ether/ethyl acetate=20:1 – 10:1), to obtain compound 1 colorless viscous liquid 8350 mg, yield 99%.

The synthetic route of 3398-16-1 has been constantly updated, and we look forward to future research findings.

Electric Literature of 82560-12-1,Some common heterocyclic compound, 82560-12-1, name is 3-Amino-5-tert-butylpyrazole, molecular formula is C7H13N3, 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.

A mixture of 2,4-dichloropyrimidine (3.73g, 25mmol) and 5-amino-3-tert-butyl-lH- pyrazole (3.55g, 25.5mmol) and DIPEA (4.44ml, 25mmol) were heated at 5O0C in TEtaF25 (75ml) for 18 hours under nitrogen. The mixture was allowed to cool and the volatiles removed by evaporation. The residue was dissolved in DCM (150ml), washed with water, dried (MgSO4) and the solvent removed by evaporation. The residue was purified by chromatography on silica gel eluting with EtOAc/hexanes (1:3) and then methanol/DCM (5:95) to give 2-chloro-4-(5-tert-butyl-lH-rhoyrazol-3-ylamino)rhoyrimidine (1.73g, 28%). NMR30 Spectrum 1.30 (s, 9Eta), 6.05 (s, IH), 7.16 (br s, IH), 8.12 (d, IH), 9.80 (br s, IH), 11.89 (br s, IH); Mass Spectrum 252 [MH]+.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3-Amino-5-tert-butylpyrazole, its application will become more common.

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. 25016-17-5, name is Methyl 5-methyl-1H-pyrazole-3-carboxylate, A new synthetic method of this compound is introduced below., Safety of Methyl 5-methyl-1H-pyrazole-3-carboxylate

Methyl 5-methylpyrazole-3-carboxylate (14 g, 0.1 mol), ethyl bromide (10.9 g, 0.1 mol),Tetrabutylammonium hydrogen sulfate (2.7 g, 0.008 mol), dissolved in 10 ml of dimethyl sulfoxide (DMSO),Potassium hydroxide solution was added dropwise [potassium hydroxide solution: a solution obtained by dissolving 22.4 g (0.40 mol) of potassium hydroxide in 20 ml of water],The reaction is exothermic, the addition is completed, and the mixture is stirred at room temperature overnight, diluted with water and quenched to adjust the pH to 2 to precipitate a white solid.Nuclear magnetic resonance test is a mixture of 1-ethyl-3-methylpyrazole-5-carboxylic acid and 1-ethyl-5-methylpyrazole-3-carboxylic acid.The ratio is 1:1, and the total weight of the product after drying is 14.6 g, and the yield is 94.8percent.

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 of 930-36-9, 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. 930-36-9, name is 1-Methylpyrazole belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

n-BuLi (2.5M in hexane, 26.8 mL, 67 mmol) was added dropwise over 15 mm to a solutionof 1-methyl-1H-pyrazole (5.0 mL, 61 mmol) in THF (100 mL) at -78 C. After stirring at-78 C for 1 h, a solution of ?2 (17 g, 67 mmol) in THF (20 mL) was added dropwise. The reaction was allowed to warm to room temperature and stirred for 1 h. The mixture wasquenched with saturated aqueous NH4C1 and poured into H20 (100 mL). The aqueous phase was extracted with Et20. The combined organic phases were washed with saturated aqueous Na2S2O3, dried over MgSO4, filtered, and concentrated under reduced pressure to afford the title compound (11.39 g, 90%).LC-MS: 208.8 [M+Hf, RT 0.94 mm. ?H NMR (500 MHz, CDC13) oe ppm 3.94 (s, 3H), 6.43 (d, J=1.97 Hz, 1H), 7.48 (d, J=2.00 Hz, 1H)

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, 1-Methylpyrazole, 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. 5334-41-8, name is 5-Amino-1-methyl-1H-pyrazole-4-carbonitrile belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below. Quality Control of 5-Amino-1-methyl-1H-pyrazole-4-carbonitrile

Alternatively, a mixture of 5 -amino- 1 -methyl- lH-pyrazolo 4-carbonitrile 2 (3.00 g, 24.59 mmol), IM aqueous solution of sodium hydroxide (1.1 equiv., 27 ml) and -30% aqueous solution of hydrogen peroxide (5 equiv., 14 ml) were stirred in methanol (30 ml) at room temperature overnight. The volume of reaction mixture was reduced in vacuo, precipitate filtered and dried to give 5 -amino- 1 -methyl- lH-pyrazolo-4-carboxylic acid amide 3 (2.99 g, 87 %).

The synthetic route of 5334-41-8 has been constantly updated, and we look forward to future research findings.

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, SDS of cas: 26621-44-3

3-Nitro-lH-pyrazole (3 g, 26.5 mmol’, 1 eq) , l-chloro-3- methylbut-2-ene (4.16 g 39.8 mmol, 1.5 eq) , potassium iodide (5 mg, 0.03 mmol, 0.001 eq. ) , and cesium carbonate (17.2 g, 53 mmol, 2 eq) were mixed in 1,4-dioxane (305 ml) . The mixture was subjected to microwave irradiation at 1200C for 30 min. The mixture was diluted with ethyl acetate and washed with water. The organic layer was dried over magnesium sulfate, filtered, and concentrated in vacuo. The residue was purified with silica gel column chromatography using 0 to 40% ethyl acetate in hexane as an eluent to give 4.18 g of the title compound (87%) as a brown oil. [M+H] calc’d for C8HnN3O2, 182 found, 182.

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.

Synthetic Route of 113100-53-1, These common heterocyclic compound, 113100-53-1, name is 1-Methyl-3-(trifluoromethyl)-1H-pyrazole-4-carboxylic acid, 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: Intermediate 5 (1.0 mmol) and 4-dimethylaminopyridine (0.1 mmol) were added to a mixture of the corresponding carboxylic acid 6 (1.3 mmol) and (EDCI, 2 mmol) in CH2Cl2 (20 mL). The reaction system was stirred at room temperature overnight and then diluted with CH2Cl2 (50 mL). The resulting mixture was consecutively washed with 10% citric acid solution and brine. Then the organic phase was dried with sodium sulphate and filtered, and concentrated under reduced pressure. The residue was purified on a silica gel column to afford the title compounds 7-17.

Statistics shows that 1-Methyl-3-(trifluoromethyl)-1H-pyrazole-4-carboxylic acid is playing an increasingly important role. we look forward to future research findings about 113100-53-1.

Related Products of 2075-46-9, 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 2075-46-9 as follows.

Intermediate 5: 1 H-Pyrazol-4-amine. 4-Nitro-1H-pyrazole (Manchester organics; 1.13 g, 9.99 mmol) was dissolved in ethanol (50 ml). This solution was added carefully to 10% palladium on carbon (Aldrich; 102 mg) under a nitrogen atmosphere. The atmosphere was exchanged to hydrogen, and the mixture was stirred vigorously at room temperature under a hydrogen atmosphere. After 45 min, ca. 700 ml of hydrogen had been taken up, and no further hydrogen was taken up over the next 30 min. Stirring was stopped and the atmosphere was exchanged to nitrogen. The solution was filtered through cellite (10 g cartridge) and washed with further ethanol (150 ml). Relevant fractions (as verified by TLC) were combined and concentrated in vacuo to give a red oil. Trituration with DCM gave the title compound (815 mg) as a red solid; 1 H NMR (MeOH-d4, 400 MHz) delta (ppm) 7.20 (2 H, s).

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.