Day: November 20, 2020

288-13-1, 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. 288-13-1 name is 1H-Pyrazole, 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.

(1) will nitroiodobenzene 0.248g (1.0mmol), pyrazole 0.069g (1.0mmol), Cu (OAc)2¡¤H2O 0.030g (0.15mmol), 2,2- biimidazole 0.022g (0.15mmol), NaOH 0.08g (2mmol), DMSO (2mL) was added the reaction tube with a piston, it was heated to 80 deg.] C the reaction was stirred for 48 hours .(2) TLC until the reaction was complete the reaction was followed ends.After the reaction was cooled to room temperature, diluted with water, extracted with ethyl acetate 3-4 was added, and the combined organic phases were dried over anhydrous sodium sulfate, filtered and concentrated to give the crude product.After the end of (3) to obtain the crude product was purified by column chromatography (petroleum ether / ethyl acetate elution) to give the desired product 7 (68% yield).

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

1192-21-8, The chemical industry reduces the impact on the environment during synthesis 1192-21-8, name is 1-Methyl-1H-pyrazol-5-amine, I believe this compound will play a more active role in future production and life.

3rd Generation BrettPhos precatalyst (11.90 mg, 0.01 mmol) was added to 1 -methyl- 1H- pyrazol-5 -amine (87 mg, 0.89 mmol), Cs2C03 (291 mg, 0.89 mmol) and (5)-2-(2-chloro-5- methylpyrimidin-4-yl)-6-methyl-7-((6-(trifluoromethyl)pyridin-2-yl)methyl)-6,7- dihydroimidazo[l,2-a]pyrazin-8(5H)-one (Intermediate 77; 130mg, 0.30 mmol) in 1,4- dioxane (5 mL) under nitrogen. The resulting mixture was stirred at 100 ¡ãC for 4 hours. The solvent was then removed under reduced pressure. The crude product was purified by flash silica chromatography, elution gradient 0 to 6percent MeOH in DCM, product containing fraction were evaporated to afford a solid. This solid was purified further by preparative HPLC (XSelect CSH Prep C18 OBD column, 5mu silica, 19 mm diameter, 150 mm length), using decreasingly polar mixtures of water (containing 0.1percent Formic acid) and MeCN as eluents. Fractions containing the desired compound were evaporated to dryness to afford (5)-6-methyl-2-(5-methyl-2-((l-methyl-lH-pyrazol-5-yl)amino)pyrimidin-4-yl)-7-((6- (trifluoromethyl)pyridin-2-yl)methyl)-6,7-dihydroimidazo[l,2-a]pyrazin-8(5H)-one (Example 27; 100 mg, 67.5percent) as a white solid. lH NMR (300 MHz, DMSO, 23 ¡ãC) delta 1.20 (3H, d), 2.56 (3H, s), 3.70 (3H, s), 4.05-4.18 (1H, m), 4.37-4.41 (1H, m), 451-4.60 (2H, m),5.212 (1H, d), 6.30 (1H, d), 7.34 (1H, d), 7.76-7.83 (2H, m), 7.96 (1H, s), 8.06-8.11 (1H, m), 8.32 (1H, s). m/z (ES+), [M+H]+ = 498.

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

120068-79-3, 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 120068-79-3 as follows.

5-Amino-3-cyano-4-dichlorofluoromethylthio-1-(2,6-dichloro-4-trifluoromethylphenyl)pyrazole, m.p. 178-180C in the form of a white solid, after purification by chromatography eluding with diethyl ether/hexane (1:1); from 5-amino-3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)pyrazole. By proceeding in a similar manner but employing a molar equivalent of pyridine in the reaction solution there was obtained:

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 120068-79-3, and friends who are interested can also refer to it.

16034-46-1, 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. 16034-46-1, name is 1-Methyl-1H-pyrazole-5-carboxylic acid belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

Oleum (1977 mmol) was slowly added to fuming nitric acid (777 mmol) followed by the addition of 2-methyl-2H-pyrazole-3-carboxylic acid (277 mmol) in small portions maintaining the reaction temperature below 60oC. Stirring at this temperature was continued for a further 1 h. On completion, the reaction mixture was poured onto crushed ice and extracted with ethyl acetate (300 mL*3). The combined organic phases were washed with water (250 mL*2) and dried over anhydrous sodium sulfate. The solvent was removed under reduced pressure to afford 2-methyl-4-nitro-2H-pyrazole-3-carboxylic acid as a light yellow solid. Compound wt: 23.6 g, 50%. 1H NMR (400 MHz, DMSO-d6) delta: 8.29 (1H, s); 3.95 (3H, s).

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

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 15366-34-4 as follows. 15366-34-4

A mixture of 3-[4-(bromomethyl)phenyl]-5-(trifluoromethyl)-1 ,2,4-oxadiazole (5.0 g, 16.3 mmol), methyl 1 H-pyrazole-3-carboxylate (3.08 g, 24.4 mmol) and potassium carbonate (3.29 g, 32.5 mmol) in acetonitrile (81 mL) was heated at 25C for 4 hours. The white suspension was filtered to remove the solids and the filtrate solution was then concentrated under reduced pressure. The resultant crude residue was purified by flash chromatography on silica gel (cyclohexane:ethyl acetate eluent gradient 99:1 to 35:65) to afford 3.90 g of the title compound as a white solid. LC/MS (Method A) retention time = 1.02 minutes, 353 (M+H). (0725) NMR (400 MHz, CDCI3) delta ppm: 8.12 (d, 2H), 7.49 (d, 1 H), 7.39 (d, 2H), 6.89 (s, 1 H), 5.51 (s, 2H), 3.98 (s, 3H). methyl 2-[[4-[5-(trifluoromethyl)-1 ,2,4-oxadiazol-3-yl]phenyl]methyl]pyrazole-3-carboxylate (Compound 5.2 of Table T5) was isolated as a byproduct in form of a white solid (1.53 g). LC/MS (Method A) retention time = 1 .1 1 minutes, 353 (M+H). (0726) NMR (400 MHz, CDCIs) delta ppm: 8.05 (d, 2H), 7.55 (s, 1 H), 7.40 (d, 2H), 6.95 (s, 1 H), 5.35 (s, 2H), 3.85 (s, 3H).

According to the analysis of related databases, 15366-34-4, the application of this compound in the production field has become more and more popular.

6126-22-3, name is 3-Amino-1H-pyrazol-5(4H)-one, 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. 6126-22-3

Scheme 3 (FIG. 17) is one synthetic pathway for preparing 6,6?-(4-nitro-1H-pyrazole-3,5- diyl)bis(3 -bromo-7-methylpyrazolo[ 1,5 -alpyrimidin-2( 1H)-one) (compound 8). Compound 8 differs from ANY1 by introduction of two additional methyl groups. Based on the crystal structure data, the methyl groups should be readily accommodated and may increase binding affinity. Briefly, pyrazol-3-one 1 is condensed with 2 to generate bicyclic 1,2-dihydropyrazolo[1,5-alpyrimidine 3. Selective bromination of 3 can be accomplished under free radical (shown) or direct bromination conditions to furnish 4. At this stage, a portion of ester 4 will undergo saponification to generate acid 5.Next, 5 is coupled to CH3NHOCH3 to yield the corresponding Weinreb amide, which can then be transformed to the corresponding methyl ketone 6 by reaction with the Grignard reagentmethyl magnesium bromide. Ester 4 and methyl ketone 6 are then coupled to yield a 1,3- dicarbonyl compound that is condensed with hydrazine to yield the pyrazole core in compound 7. Finally, mild nitration with copper (II) nitrate will deliver compound 8, a direct analogue of ANY 1

Statistics shows that 6126-22-3 is playing an increasingly important role. we look forward to future research findings about 3-Amino-1H-pyrazol-5(4H)-one.

1145-01-3, 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. 1145-01-3 name is 3,5-Diphenyl-1H-pyrazole, 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 solution of 3,5-diphenyl-1H-pyrazole (0.36 g, 1.65 mmol) in N,N-dimethylformamide (8.6 mL) was added sodium hydride (60% in oil, 66 mg, 1.65 mmol) under stirring at room temperature, and the mixture was stirred at the same temperature for 30 min. To the reaction mixture was added sodium iodide (22 mg, 0.15 mmol) and a solution of methyl 4-(bromomethyl)-3-isopropoxybenzoate (0.43 g, 1.50 mmol) in N,N-dimethylformamide (4.3 mL), and the mixture was stirred at room temperature for 3 hr. The reaction mixture was diluted with ethyl acetate, washed with water and saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=10/1-hexane/ethyl acetate=4/1) to give the title compound (0.59 g, yield 92%) as a colorless oil. MS (ESI+): 427 (M+H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3,5-Diphenyl-1H-pyrazole, and friends who are interested can also refer to it.

5932-32-1, A common compound: 5932-32-1, name is 1,4,5,6-Tetrahydrocyclopenta[c]pyrazole-3-carboxylic acid, 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.

To a mixture of 1,4,5,6-tetrahydrocyclopenta[c]pyrazole-3-carboxylic acid (A-3) (2.50 g, 16.43 mmol) in DMF (16.43 ml) at ambient temperature were added TEA (2.75 ml, 19.72 mmol), HATU (7.50 g, 19.72 mmol), and (2R,6S)-2,6-dimethylmorpholine (2.84 g, 24.65 mmol). The mixture stirred for 3 h before acidifying with AcOH (5 mL). The mixture was purified directly by column chromatography on C18 column (5-95% ACN/water with 0.05% TFA modifier) to afford the title compound. MS: 250.3 (M+1).

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, 1,4,5,6-Tetrahydrocyclopenta[c]pyrazole-3-carboxylic acid, other downstream synthetic routes, hurry up and to see.

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. 4522-35-4, name is 3-Iodo-1H-pyrazole, A new synthetic method of this compound is introduced below., 4522-35-4

Step B: 3-(ter?-Butoxy)-5-(3-iodo-lH-pyrazol-l-yl)pyridazine To a solution of 3-iodopyrazole (0.208 g, 1.072 mmol) in DMF (5.36 mL) was added potassium teri-butoxide (0.132 g, 1.179 mmol) and then stirred at room temperature for 10 min. 3-(t

Adding some certain compound to certain chemical reactions, such as: 5952-92-1, name is 1-Methyl-1H-pyrazole-4-carboxylic acid, 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 5952-92-1. 5952-92-1

A suspension of 1 -methyl- lH-pyrazole-4-carboxy lie acid (0.25 g) in thionyl chloride (4 mL) was stirred at reflux for 30 minutes. The reaction was concentrated, the residue azeotroped with toluene and dissolved in acetonitrile (5 mL). To the cooled (0 ¡ãC) solution, a 2 M solution of (trimethylsilyl)diazomethane in hexanes (1.5 mL) was added and the mixture stirred at 0 ¡ãC for 1 hour. A solution of 33 wt. percent hydrogen bromide in acetic acid (1.0 mL) was added and the mixture stirred at room temperature for a further 80 minutes. To the reaction mixture, tert-butyl methyl ether (20 mL) was added and the resultant precipitate isolated by filtration to give the title product having the following physical properties (0.22 g). LC MS rR 1.23 minutes; MS (ES+) m/z 203 and 205 (M+H) a.

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 1-Methyl-1H-pyrazole-4-carboxylic acid.