Month: May 2021

Related Products of 113402-89-4, 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 113402-89-4 as follows.

Will 10mmol compound 1,10 mmol of compound 2 and 1 mmol of K2CO3 and 10 mL of PEG 400 were added to the reaction flask.Reaction at 80 ° C for 24 h,The reaction solution was cooled to room temperature.Precipitating in ether,The filtrate was collected by filtration.Purified by gel chromatography (mobile phase petroleum ether / ethyl acetate = 5:1),Compound 3;Compound 3 (1 mmol),Raney Nickel (0.1g),Sodium n-propoxide (0.92 g, 11 mmol) was dissolved in 50 mL of 1,2-dimethoxyethane.Reaction at 60 ° C for 10 h,Cool to room temperature,Collect organic phase by filtration,Removal of 1,2-dimethoxyethane by rotary evaporation,The compound 62 was purified by column chromatography using acetonitrile / dichloromethane (5:1 by volume).

According to the analysis of related databases, 113402-89-4, the application of this compound in the production field has become more and more popular.

Synthetic Route of 52867-42-2, A common heterocyclic compound, 52867-42-2, name is Methyl 2-methyl-5-oxo-2,5-dihydro-1H-pyrazole-3-carboxylate, molecular formula is C6H8N2O3, 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.

Cyclopropanol (413 mg, 6.40 mmol) and methyl 5-hydroxy-2-methyl-pyrazole-3-carboxylate (1.0 g, 6.40 mmol) were suspended in anhydrous toluene (10.0 mL) prior to addition of triphenylphosphine (1.69 g, 6.40 mmol) and then di-tert-butylazodicarboxylate (1.47 g, 6.40 mmol). The reaction was heated to 110 C with stirring in a sealed vessel for 4.5 h, cooled & diluted with EtOAc (10 mL) and washed with water (10 mL). The organic layer was dried over Na2S04 and concentrated in vacuo. The crude product was purified by column chromatography eluting with a 0-100% gradient of EtOAc in isohexane. Product-containing fractions were combined and concentrated to afford the title compound (730 mg, 58% Yield). 6H (300 MHz, Chloroform-d) 6.31 (s, 1H), 4.04 (s, 3H), 3.91 (tt, J = 6.0, 3.0 Hz, 1H), 3.86 (s, 3H), 0.82 – 0.66 (m, 4H).

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.

Application of 28466-26-4, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 28466-26-4 name is 4-Aminopyrazole, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

As shown in step 6-iii of Scheme 6, lH-pyrazol-4-amine (149 mg, 1.79 mmol), methyl 2-(bromomethyl)-4-(5,6-dimethoxy-3-pyridyl)-6-methyl-benzoate (680 mg, 1.79 mmol) and DIEA (231 mg, 312 mu^, 1.79 mmol) were combined in DMF (5 mL), heated to 90C for 6 hours, and allowed to cool to room temperature over 16 hours. The reaction mixture was taken up in EtO Ac/water and the organic layer washed with water, brine, dried, and concentrated under reduced pressure to yield a foam. The foam was recrystallized in DCM/MeOH. The resulting solid was collected by filtration, washed with DCM, and dried under vacuum to provide 5-(5,6-dimethoxy-3-pyridyl)-7-methyl-2-(lH-pyrazol-4- yl)isoindolin-l-one (Compound 2024, 115 mg). The filtrate from the recrystallization was concentrated under reduced pressure and the residue purified by silica gel chromatography (20 to 100% EtO Ac/hex) to yield an additional 88 mg of Compound 2024 (total yield 203 mg, 0.66 mmol, 32% yield): ESMS (Mu+Eta) 351.26; 1H NMR (DMSO-d6) delta 12.83 (s, 1Eta), 8.10 (m, 2Eta), 7.88 (s, 1Eta), 7.74 (s, 1Eta), 7.61 (s, 2Eta), 4.83 (s, 2Eta), 3.92 (s, 3Eta), 3.91 (s, 3Eta), 2.72 (s, 3Eta).

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

Adding a certain compound to certain chemical reactions, such as: 288-13-1, name is 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 288-13-1, COA of Formula: C3H4N2

4-Iodopyrazole (20) A flask equipped with a nitrogen inlet, an addition funnel, a thermowell, and a mechanical stirrer was charged with pyrazole (1, 450 g, 6.62 mol) and tetrahydrofuran (THF, 5 L) at ambient temperature. The mixture was then cooled to 10 C. and N-iodosuccinimide (NIS, 1490 g, 6.62 mol, 1.0 equiv) was added to the mixture in portions as a solid at approximately 10 C. The resulting reaction mixture was then stirred at ambient temperature for 1 hour (longer reaction times may be necessary depending on ambient temperature). The mixture was then filtered and the THF was removed under reduced pressure. The residue was suspended in ethyl acetate (6 L) and insoluble materials were filtered. The dark filtrate was sequentially washed with saturated aqueous sodium thiosulfate solution (2*3 L) (organic layer lightens to a pale yellow), water (2*3 L), and brine (2 L). The resulting organic layer was then dried over sodium sulfate, filtered, and concentrated under reduced pressure to afford 4-iodopyrazole (1138 g, 1284.1 g theoretical, 88.6%) as a white to pale yellow solid after being dried in a vacuum oven at approximately 30 C. overnight. 1H NMR (400 MHz, DMSO-d6) delta 13.17 (bs, 1H), 7.93 (bs, 1H), 7.55 (bs, 1H) ppm; C3H31N2 (MW, 193.97), LCMS (EI) m/e 195 (M++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.

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 35277-02-2 as follows. SDS of cas: 35277-02-2

Step 1 : Benzyl 1-(4-fluoro-1 H-pyrazol-1 -yl)cyclopropanecarboxylate To a solution of 4-fluoropyrazole (125 mg, 1.45 mmol) in tetrahydrofuran (4 mL) at 0C was added sodium hydride (60% suspension in mineral oil, 1 16 mg, 2.90 mmol). The mixture was stirred at 0C for 40 min before benzyl 2,4-dibromobutyrate (0.30 mL, 1.50 mmol) was added dropwise. The reaction mixture was stirred at room temperature for 18 h. The reaction mixture was diluted with ethyl acetate and washed with water and brine. The organics were dried over sodium sulfate, filtered and concentrated under reduced pressure. The residue was purified via flash chromatography to afford benzyl 1-(4-fluoro-1 /-/-pyrazol-1-yl)cyclopropanecarboxylate as a clear oil (1 15 mg, 30.4%). 1H NMR (400 MHz, CDCI3) delta 1.64-1.70 (m, 2H), 1.81 -1.86 (m, 2H), 5.14 (s, 2H), 7.22-7.26 (m, 2H), 7.31-7.36 (m, 3H), 7.40 (td, 2H).

According to the analysis of related databases, 35277-02-2, the application of this compound in the production field has become more and more popular.

Related Products of 13745-17-0, 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 13745-17-0 as follows.

General procedure: The fragment carboxylic acid (0.35 mmol) was dissolved in dimethylformamide (0.2 M, 1.75 mL), then 14 (42.6 mg, 0.35 mmol), HBTU (128 mg, 0.34 mmol), and HOBT (51.8 mg, 0.38 mmol) were added, followed by diisopropylethylamine (175 muL, 1.047 mmol). The reaction was stirred at 23 C for 16 h. TLC at 16 h showed conversion to product. The reaction was quenched with H2O (5 mL) and extracted with DCM (3 x 5 mL). The combined organic layers were washed with 1 M HCl (10 mL), saturated aqueous NaHCO3 (10 mL), and saturated aqueous NaCl (10 mL). The organic layer was dried over MgSO4, filtered, and evaporated. Purification with flash column chromatography with CH3OH/CH2Cl2 ( CH3OH gradient 0 ? 5 %).

According to the analysis of related databases, 13745-17-0, the application of this compound in the production field has become more and more popular.

Synthetic Route of 133228-21-4,Some common heterocyclic compound, 133228-21-4, name is N,N-Dimethyl-1H-pyrazole-1-sulfonamide, molecular formula is C5H9N3O2S, 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.

Step A: Preparation of 3-Chloro-N,N-dimethyl-1H-pyrazole-1-sulfonamideTo a solution of N-dimethylsulfamoylpyrazole (188.0 g, 1.07 mol) in dry tetrahydrofuran (1500 mL) at -78 C. was added dropwise a solution of 2.5 M n-butyllithium (472 mL, 1.18 mol) in hexane while maintaining the temperature below -65 C. Upon completion of the addition the reaction mixture was maintained at -78 C. for an additional 45 minutes, after which time a solution of hexachloroethane (279 g, 1.18 mol) in tetrahydrofuran (120 mL) was added dropwise. The reaction mixture was maintained for an hour at -78 C., warmed to -20 C. and then quenched with water (1 L). The reaction mixture was extracted with methylene chloride (4×500 mL); the organic extracts were dried over magnesium sulfate and concentrated. The crude product was further purified by chromatography on silica gel using methylene chloride as eluent to afford the title product compound as a yellow oil (160 g). 1H NMR (CDCl3) delta 3.07 (d, 6H), 6.33 (s, 1H), 7.61 (s, 1H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route N,N-Dimethyl-1H-pyrazole-1-sulfonamide, its application will become more common.

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., COA of Formula: C5H9N3

General procedure: A mixture of 5-amino-3-methylpyrazole (1 mmol), isatin or acenaphthylene-1,2-dione (1 mmol), thioacid (1 mmol), and p-TSA (30 mol %) in CH3CN (5 mL) was stirred at 80 C for 12-24 h. After completion of the reaction confirmed by TLC (eluent acetone/petroleum ether, 1:2), the reaction mixture was cooled to room temperature. Then, the solvent was removed under vacuum. The solid was recrystallizated from CH3CN and ethanol to afford the pure 4 or 6 as a white or yellow powder.

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.

Adding a certain compound to certain chemical reactions, such as: 176969-34-9, name is 3-(Difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid, 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 176969-34-9, COA of Formula: C6H6F2N2O2

To 176 mg of 3-difluoromethyl-1-methyl-1 H-pyrazole-4-carboxylic acid in 1 ml of dichloromethane, 10 mg of N,N-dimethylformamide and 381 mg of oxalyl chloride were added, and the mixture was stirred at room temperature for 1 hour. After completion of the reaction, the solvent was evaporated under reduced pressure, and the resulting residue was dissolved in 2 ml of dichloromethane, and to the solution, 190 mg of the 2-amino-1-(3,5-dichloropyridin-2-yl)ethanone-O-ethyloxime prepared in Step 5 in Synthetic Example 2 in 2 ml of dichloromethane and then 91 mg of pyridine were added dropwise with stirring under cooling with ice, and after the addition, the mixture was stirred at room temperature for another 2 hours. After completion of the reaction, the reaction mixture was mixed with 10 ml of water and extracted with chloroform (20 ml*1), the resulting organic layer was washed with water (10 ml*1) and dried over saturated aqueous sodium chloride and then anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography using ethyl acetate-hexane (with a gradient of from 1:4 to 1:1) as the eluent to obtain 165.3 mg of a pale yellow resinous substance. The resinous substance was dissolved in 5 ml of acetic acid and stirred at 70C for 2 hours, the solvent was evaporated under reduced pressure, and the resulting residue was purified by silica gel column chromatography using ethyl acetate-hexane (with a gradient of from 1:4 to 1:1) as the eluent to obtain 130.6 mg of the desired product as a colorless resinous substance (E/Z=1/1). 1H NMR (CDCl3, Me4Si, 300MHz) delta8.50 and 8.47 (d, J=2.1 Hz, 1 H), 7.90 and 7.86 (s, 1H), 7.76 and 7.75 (d, J=2.1Hz, 1H), 6.9-7.1 (m, 1H), 6.84 and 6.73 (t, J=54.3Hz, 1H), 4.71 and 4.49 (d, J=6.0Hz, 2H), 4.31 and 4.14 (q, J=7.2Hz, 2H), 3.92 and 3.89 (s, 3H), 1.36 and 1.23 (t, J=7.2Hz, 3H).

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.

113100-53-1, name is 1-Methyl-3-(trifluoromethyl)-1H-pyrazole-4-carboxylic acid, 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. COA of Formula: C6H5F3N2O2

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.

The synthetic route of 113100-53-1 has been constantly updated, and we look forward to future research findings.