Tag: M.W:200-300

83-10-3, 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. 83-10-3 name is 1,5-Dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazole-4-carboxylic acid, 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.

Step 2) N-(2-fluoro-4-hvdroxyphenyl)-L5-dimethyl-3-oxo-2-phenyl-2,3-dihvdro-lH- pyrazole-4-carboxamide [0205] To a suspension of 4-amino-3-fluorophenol (1.0 g, 7.87 mmol) and 1,5- dimethyl-3-oxo-2-phenyl-2,3-dihydro-lH-pyrazole-4-carboxylic acid (2.19 g, 9.44 mmol) in CH2C12 (20 mL) were added EDCI (3.02 g, 15.7 mmol) and HOAT (0.21 g, 1.57 mmol). The reaction mixture was refluxed for 20 hours, and then cooled to rt. Water (10 mL) was added and the mixture stirred at rt overnight, then filtered and the filter cake was washed with water (5 mL), followed by purifying by a silica gel column chromatography (CH2Cl2/MeOH (v/v) = 70/1) to give the title compound as a beige white solid (1.25 g, 46.6%). MS (ESI, pos, ion) m/z: 342.1 [M+H]+, Rt = 2.712 min.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,5-Dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazole-4-carboxylic acid, and friends who are interested can also refer to it.

39806-90-1, The chemical industry reduces the impact on the environment during synthesis 39806-90-1, name is 4-Iodo-1-methyl-1H-pyrazole, I believe this compound will play a more active role in future production and life.

e-2) Preparation of [0250] [0251] N2 atmosphere. A mixture of intermediate (62) (0.004 mol), 4-iodo-1-methyl-1H-pyrazole (0.0035 mol), 1,4-dioxane (25 ml) and Cs2CO3 (1.6 g) in Xantphos (0.1 g) was degassed. Pd2(dba)3 (0.13 g) was added and the reaction mixture was degassed again. The reaction mixture was stirred at 80-90 C. for 2 hours. After cooling, the reaction mixture was filtered over dicalite. The filtrate was concentrated and the residue was purified on silica gel using DCM/CH3OH (from 100% to 96/4) as eluent. The product fractions were collected and evaporated to dryness. The residue was used as such in the next reaction, yielding 0.14 g of intermediate (64).

The chemical industry reduces the impact on the environment during synthesis 39806-90-1. I believe this compound will play a more active role in future production and life.

A common compound: 18048-64-1, name is 1-(3,4-Dimethylphenyl)-3-methyl-1H-pyrazol-5(4H)-one, 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. 18048-64-1

4- (7-amino-6-hydroxy-2,3-dihydro-1H – inden-5-yl) benzoic acid hydrobromide(0.5g, 1.43mmol) was dissolved in 15ml of concentrated hydrochloric acid, cooled to 0 , theretowas slowly added dropwise of NaNO2(0.11 g of, 1.51 mmol) aqueous solution (10ml), the reaction incubated0.5h, TLC detection starting material the reaction was complete.Thereto was added 1- (3,4-dimethylphenyl) -3-methyl-1H – pyrazol-5 (4 hydrogen) -one (0.29g, 1.43mmol), the reaction 15min,controlling the reaction temperature is 0 deg.] C, with saturated sodium bicarbonate to adjust the pH value of about 9, was added 10mlof absolute ethanol, naturally to room temperature after the reaction was continued for 24h, TLC detection starting material the reaction was complete,filtered and the resulting cake was washed with 40ml of hydrochloric acid solution (concentration of 2mol / L) washed several times with methanolpulping, beating dichloromethane, filtration give (Z) -4- (7- (2- (1- (3,4-dimethylphenyl) -3-methyl-5-oxo substituting 1,5-dihydro – pyrazol-4-ylidene) hydrazino-yl) -6-hydroxy-2,3-dihydro -1H-indan-5-yl) benzoic acid (0.33mg, yield 44 %).

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, 18048-64-1, other downstream synthetic routes, hurry up and to see.

330792-70-6, 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. 330792-70-6 name is 3-Amino-5-(4-phenoxyphenyl)pyrazole-4-carbonitrile, 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.

To a dry 10 L three-necked flask was added Compound 1a (600 g, 2.17 mol)Compound 2a (815 g, 2.39 mol),Powdered cesium carbonate (1417 g, 4.35 mol) and N, N-methylformamide (DMF, 6 L) were added,Mechanical stirring, heating the internal temperature rose to 80 (about 1.5 hours)After 2 hours to send HPLC monitoring reaction, the reaction is complete, stop heating, cooled to room temperature,Then add 10L ethyl acetate and 15L water, stirred for 30 minutes (speed 200), allowed to stand,Liquid separation, the water phase to discard, the organic phase with 1kg anhydrous sodium sulfate and stir, filtered,The filtrate was concentrated dark reddish brown oil, the crude product was recrystallized twice with dioxane,Obtained pale yellow powdery solid 450g, yield 46.4percent.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3-Amino-5-(4-phenoxyphenyl)pyrazole-4-carbonitrile, and friends who are interested can also refer to it.

39806-90-1, 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. 39806-90-1, name is 4-Iodo-1-methyl-1H-pyrazole, This compound has unique chemical properties. The synthetic route is as follows.

To 4-iodo-1-methyl-1 H-pyrazole (1.0346 g, 4.97 mmol) in THF (20 ml) was added CuI (0.36g, 1.89 mmol), and PdCI2(PPh3J2. The reaction flask was purged with N2 and NEt3 (10.4 ml_, 75 mmol) and ethynyl-trimethyl-silane (5.27 ml, 37 mmol) was added. The reaction mixture was heated at 80 0C overnight for 21 hours. After cooling to room temperature, the reaction was diluted with EtOAc and filtered. The filtrate was washed successively with 1 M HCI, 1 M NaOH and H2O. The organic phase was dried over MgSO4, filtered and concentrated in vacuo. The crude product was purified by column chromatography (20:8 v/v petroleum ether : EtOAc to give the product as a brown oil (676 mg).

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.

1145-01-3, Adding some certain compound to certain chemical reactions, such as: 1145-01-3, name is 3,5-Diphenyl-1H-pyrazole, 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 1145-01-3.

A solution of ethyl 3,5-diphenyl-1-hydro-pyrazole (0.20 mmol ), alpha-benzyl diazoacetoacetate ( 0.25 mmol) was added in a 2 5 mL Schrocker tube at room temperature.[Cp * RhCl2] 2 (0¡¤01 mmol), AgSbF6 (0.04 mmol) and tetrahydrofuran (2.00 mL) were added and argon was bubbled through argon for 2 minutes. Stir at 25 C for 48 hours. The reaction was stopped and concentrated under reduced pressure to give a crude product. Finally, the mixture was washed with a mixture of petroleum ether and ethyl acetate, and the corresponding nitrogen-containing fused heterocyclic compound (77 mg of white solid, 99% yield) was obtained by flash column chromatography (baby gel column).

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 1145-01-3.

A common heterocyclic compound, 141573-95-7, name is Ethyl 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylate, molecular formula is C8H10F2N2O2, 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. 141573-95-7.

The azinium salt (10.0 g, 29.9 mmol) was suspended in 50 mL of toluene. A solution of NaOH (1.44 g, 36.0 mmol) in 50 mL of water was added and the biphasic mixture was heated to 60 C. for 3 h. The mixture was then cooled to rt, the phases split and the aqueous phase extracted with 20 mL of toluene. The combined org. phases were used in the next step without further purification. To the solution of the aminal in toluene were added ethyl alpha-ethoxymethylene-4,4-difluoro-3-oxobutyrate (6.64 g, 29.9 mmol) and p-TsOH monohydrate (0.57 g, 3.0 mmol). The solution was stirred overnight at rt, then heated to 60 C. for one hour. The solution was then cooled to it and extracted with 30 mL sat. NaHCO3 solution. The org. phase was used in the next step without further purification. To the org. phase was added 10% KOH solution (24.1 g). The biphasic mixture was heated to 60 C. and the disappearance of the ester monitored by GC. When the ester had completely vanished, the solution was cooled to rt. The phases were then split and the aqueous phase was heated to 55 C. Then, 30% H2SO4 solution (16 g) were added and stirring continued for 60 min. The solution was then cooled to 5 C. and the precipitated product removed by filtration. The precipitate was washed with cold water and dried under reduced pressure overnight (p<20 mbar, 50 C.). The product was obtained as a yellow powder (2.87 g, 16.3 mmol, 55% yield based on the azinium salt). 1H NMR (500 MHz, DMSO-d6): delta (ppm)=8.33 (s, 1H); 7.22 (t, J=54 Hz, 1H); 3.93 (s, 3H). 13C NMR (125 MHz, DMSO-d6): delta (ppm)=163.0; 145.1 (t, J=24 Hz); 136.1; 113.0 (t, J=3 Hz); 109.6 (t, J=234 Hz); 39.2. 19F NMR (470 MHz, DMSO-d6): delta (ppm)=-126.0 (d, J=54 Hz). mp=205 C. Purity (cal. HPLC): 97.1% (0.4% iso-DFP acid) The synthetic route of Ethyl 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylate has been constantly updated, and we look forward to future research findings.

A common heterocyclic compound, 1145-01-3, name is 3,5-Diphenyl-1H-pyrazole, molecular formula is C15H12N2, 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. 1145-01-3.

EXAMPLE 5 The preparation of 1 -methyl-3,5-diphenylpyrazole Five parts of 3,5-diphenylpyrazole are dissolved in 25 parts (by volume) of methyl isobutyl ketone. Solid anhydrous sodium hydroxide (1.1 parts) is added and the mixture is heated to 90C. Dimethyl sulfate (3.43 parts) is added and the mixture is next heated to 112C. to 115C. The reaction mixture is sampled after 1.5 hours, and no unreacted 3,5-diphenylpyrazole is found to be present. The reaction mixture is cooled to 50C., and 30 parts of water are added. The pH is next adjusted to between 11 and 12 by the addition of aqueous sodium hydroxide. The organic layer is washed twice with 30 parts water. For yield determination the methyl isobutyl ketone is removed in vacuo, producing 4.95 parts (93% crude yield) of an oil which crystallizes on cooling (melting point 52C. to 53C). Analysis of the product shows it to be 85.5% pure as 1-methyl-3,5-diphenylpyrazole.

The synthetic route of 3,5-Diphenyl-1H-pyrazole has been constantly updated, and we look forward to future research findings.

39806-90-1, Adding some certain compound to certain chemical reactions, such as: 39806-90-1, name is 4-Iodo-1-methyl-1H-pyrazole, 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 39806-90-1.

To a solution of 4-iodo-l-methyl-lH-pyrazole (153 mg, 0.736 mmol) in anhydrous DMSO (15 ml) was added intermediate 20.1-1 (190 mg, 0.613 mmol), (Irans)-N 1.N2-dimethylcyclohexane- 1, 2-diamine (34.9 mg, 0.245 mmol), potassium phosphate (391 mg, 1.840 mmol) and Cul (23.36 mg, 0.123 mmol). The resulting mixture was stirred at 90C under N2 protection for 12 hours. After cooling to room temperature, filtering and concentrating, the crude material was purified by pre-HPLC (TFA) to give example 20.2-1, ( R,R or 5′,5′)-5-chloro-6-(3-nuoro- 1 -(oxetan-3- yl)piperidin-4-yl)-l-(l-methyl-lH-pyrazol-4-yl)-lH-indazole, TFA salt. MS (ESI) m/z calc?d for C19H22CIFN5O [M+H]+ 390, found 390. NMR (400 MHz, CD3OD) d 8.17 (s, 2H), 7.96 (s, 1H), 7.88 (s, 1H), 7.65 (s, 1H), 5.16-5.41 (m, 1H), 4.76-4.86 (m, 4H), 4.36 (q, J = 6.36 Hz, 1H), 4.01 (s, 3H), 3.69-3.85 (m, 2H), 3.41 (m, 1H), 2.85-3.03 (m, 2H), 2.27 (m, 1H), 1.95-2.11 (m, 1H). LRRK2 IC50 1.7 nM.

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 39806-90-1.

39806-90-1, Adding a certain compound to certain chemical reactions, such as: 39806-90-1, name is 4-Iodo-1-methyl-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 39806-90-1.

General procedure: 4-Iodo-1-methyl-1H-pyrazole 1 (101 mg, 0.5 mmol) and phenylboronic 2 (59 mg, 0.5 mmol) were dissolved in DME (3 mL) and H2O (1.2 mL) in a microwave vial under a nitrogen atmosphere. Pd(PPh3)4 (2 mmol%, 11.6 mg) and Cs2CO3 (407.3 mg, 1.25 mmol) were added, and the reaction mixture was irradiated in a microwave apparatus at 90 C for 5-12 min. After the reaction mixture was cooled to ambient temperature, the product was concentrated, and the crude mixture was purified by silica gel column chromatography using petroleum ether/acetone as eluent to give the title compound.

According to the analysis of related databases, 39806-90-1, the application of this compound in the production field has become more and more popular.