Category: 176969-34-9

Synthetic Route of 176969-34-9, These common heterocyclic compound, 176969-34-9, name is 3-(Difluoromethyl)-1-methyl-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.

Will be 18 grams (0.1 mole)3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acidAdd 30 ml of toluene10 drops of DMF, 30 g (0.25 mol) of thionyl chloride was added dropwise at room temperature.Then, the temperature was refluxed for 5 hours.Remove the solvent by rotary evaporator to get reddish brown3-(Difluoromethyl)-1-methyl-1H-pyrazole-4-carbonyl chloride.

The synthetic route of 176969-34-9 has been constantly updated, and we look forward to future research findings.

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. 176969-34-9, name is 3-(Difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid, A new synthetic method of this compound is introduced below., Product Details of 176969-34-9

The compound of formula (III) was added to a 5% aqueous solution of sodium hydroxide, reacted at 60 C for 3 hours, and then hydrochloric acid was added to neutralize the pH to a weak acidity,(IV) 1-methyl-3-difluoromethyl-1H-pyrazole-4-carboxylic acid;The compound of formula (IV) (40 mmol) was refluxed with thionyl chloride (0.4 mol) for 4 hours and distilled under reduced pressure to give(V) 1-methyl-3-difluoromethyl-1H-pyrazole-4-carbonyl chloride;

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.

Related Products of 176969-34-9,Some common heterocyclic compound, 176969-34-9, name is 3-(Difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid, molecular formula is C6H6F2N2O2, 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 3-(difiuoromethyl)-l-methyl-lH-pyrazole-4-carboxylic acid (0.25 g, 1.42 mmol) and thionyl chloride (5 mL) was heated to reflux for 1 h. The cooled reaction mixture was concentrated under reduced pressure and the resulting residue was twice diluted with toluene and concentrated under reduced pressure. The residual 3 -(difiuoromethyl)- 1-methyl- lH-pyrazole-4-carbonyl chloride was taken up in dichloromethane (5 mL) and treated dropwise at room temperature with a mixture of 6-chloro-N-cyclopropyl-a-methyl-3- pyridinemethanamine (i.e. the product of Step A, 0.23 g, 1.18 mmol) and triethylamine (0.12 g, 1.18 mmol) in dichloromethane. The reaction mixture was stirred overnight at ambient temperature, and then partitioned between IN hydrochloric acid and dichloromethane. The organic phase was separated and the aqueous phase extracted again with dichloromethane. The combined organic phases were dried (MgSC^) and concentrated under reduced pressure. The residue was chromatographed on silica gel eluting with 30 to 100% ethyl acetate in hexanes to yield the title compound (0.27 g). in NMR delta 8.39 (m, 1H), 7.65 (m, 2H), 7.28 (d, 1H), 7.01 (t, 1H), 5.68 (m, 1H), 3.96 (s, 3H), 2.62 (m, 1H), 1.79 (d, 3H), 0.64 (m, 2H), 0.52 (m, 1H), 0.35 (m, 1H).

The synthetic route of 176969-34-9 has been constantly updated, and we look forward to future research findings.

176969-34-9, 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. 176969-34-9, name is 3-(Difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid, A new synthetic method of this compound is introduced below.

The pyrazole acid chloride is prepared from 3- difluoromethyl-1-methyl-1H-pyrazole-4-carboxylic acid and thionyl chloride in heptane shortly before use. In a 500-mL round-bottomed flask provided with alkaline scrubber, pyrazole acid (74.0 grams, 0.42 mol) is suspended in heptane (170 mL) . Dimethylformamide (0.70 grams, 0.009 mol) and thionyl chloride (55.0 grams, 0.462 mol) are added and the bi-phasic mixture is stirred and heated at 42-45 C.After complete conversion of pyrazole acid (2.5 hours), the solvent and excess thionyl chloride are completely removed by vacuum distillation.Liquid pyrazole acid chloride is obtained as the residue (approximately 81.0 grams)

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176969-34-9,Some common heterocyclic compound, 176969-34-9, name is 3-(Difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid, molecular formula is C6H6F2N2O2, 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: Under nitrogen atmosphere, carboxylic acid II (3mmol), EDCI (3.3 mmol), HOBT (3.3 mmol)and Et3N (1.8 mmol) were placed in a three-necked flask with 40 mL CH2Cl2, and stirred for 2 hat 0 C; then, compound I (2.4 mmol) was added to the flask and allowed to react for 3 h at 0 C.The reaction was monitored by thin-layer chromatography (TLC) (all reactions could be completed in3 h) and, on completion of the reaction, the mixture was washed with saturated NaHCO3 solutionand water, respectively. Then, it was dried over anhydrous Na2SO4, filtered and evaporated onrotavapor in vacuum. Subsequently, crude products III-1-III-18 were purified by silica gel columnchromatography [V (CH2Cl2): V (EA) = 3:1] and crude products III-19-III-36 were purified by silicagel column chromatography [V (PE): V (EA) = 3:1]. Finally, products were recrystallized with thedichloromethane/petroleum ether to obtain pure target compounds.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3-(Difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid, its application will become more common.

The chemical industry reduces the impact on the environment during synthesis 176969-34-9, name is 3-(Difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid, I believe this compound will play a more active role in future production and life. 176969-34-9

3 -(difluorochloromethyl)-l -methyl- lH-pyrazol-4-carboxylic acid obtained by example 5 is treated with oxalyl chloride (1,25 eq) in toluene, and a few drops of dimethylformamide are added. The mixture is concentrated under reduced pressure to yield the carboxyl chloride.

The chemical industry reduces the impact on the environment during synthesis 176969-34-9. I believe this compound will play a more active role in future production and life.

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. 176969-34-9, name is 3-(Difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid, This compound has unique chemical properties. The synthetic route is as follows., 176969-34-9

At room temperature under a nitrogen atmosphere, 14.0 parts of 1-methyl-3-difluoromethylpyrazole-4-carboxylic acid and 35.1 parts of xylene were mixed. The obtained mixture was heated at 100 C. To the obtained mixture was added dropwise 11.2 parts of thionyl chloride over 5 hours. The obtained mixture was stirred at 100 C. for 15 hours and then cooled to 40 C. Thionyl chloride and xylene were evaporated from the obtained reaction mixture under reduced pressure to obtain brown 1-methyl-3-difluoromethylpyrazole-4-carboxylic acid chloride.

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.

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.

176969-34-9, These common heterocyclic compound, 176969-34-9, name is 3-(Difluoromethyl)-1-methyl-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.

1-methyl-3-difluoromethyl-1H-pyrazole-4-carboxylic acid (7.76 g, 40 mmol) represented by formula (III) was refluxed with thionyl chloride (47.6 g, 0.4 mol) for 4 hours. When the reaction system turns to a pale yellow transparent liquid, the reaction is continued for 30 min. The reaction is stopped, and after cooling down to room temperature, 1-methyl-3-difluoromethyl-1H-pyrazole-4-acyl chloride is obtained by distillation under reduced pressure. 1-methyl-3-difluoromethyl-1H-pyrazole-4-carbonyl chloride (2 mmol) was added to 15 ml of dichloromethane, Phenylmethanamine (2.1 mmol) was added followed by slow triethylamine (0.3 g, 3 mmol) stirring overnight at room temperature; followed by TLC (EA:PE=2:1 (V)) until the reaction was complete with dichloromethane. Three times extraction with water=1:1 (V) system, concentration of organic layer, extraction with toluene or 75% ethanol, and column chromatography (EA:PE=2:1(V)) to obtain N-benzyl as shown in (K11). 1-Methyl-3-(difluoromethyl)-1H-pyrazole-4-carboxamide

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 176969-34-9.

A common heterocyclic compound, 176969-34-9, name is 3-(Difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid, molecular formula is C6H6F2N2O2, 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. 176969-34-9.

3-(difluoromethyl)-1 -methyl-i H-pyrazole-4-car-boxylic acid (2 g, 11.36 mmol) was dissolved in 20 mL sulthryl dichloride, and then heated to reflux for 3 h, the excessive sulfuryl dichloride was evaporated under reduced pressure to get 3-(difluoromethyl)-i -methyl- iH-pyrazole-4- carbonyl chloride, and then the carbonyl chloride was dissolved in 30 mL dichloromethane for the following reaction. To a cooled solution of (3-aminophenyl)methanol (1.4 g, 11.36 mmol) dissolved in 20 mL dichloromethane and 5 mL triethylamine was added slowly the solution of the carbonyl chloride at 0-5 C. Afier the reaction was stirred for 6 h at room temperature, analysis by Thin-Layer Chromatography showed complete conversion to product, the excessive solvent was evaporated under reduced pressure. the residual was purified by column chromatography on silica gel (eluent: ethyl acetate:petroleum ether=i:3; silica gel: 100-140 mesh, Qingdao Marine Chemical Co., Ltd.) to obtain 3-(di- fluoromethyl)-N-(3-(hydroxymethyl)phenyl)- i-methyl-i Hpyrazole-4-carboxamide (2.32 g) as white solid with yield of 73%. ?H NMR (300 MHz, CDC13) oe (ppm): 4.11 (s, 3H),4.73 (s, 2H), 7.16-7.81 (m, 6H).

The synthetic route of 3-(Difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid has been constantly updated, and we look forward to future research findings.