Category: 288-13-1

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.

The chemical industry reduces the impact on the environment during synthesis 288-13-1, name is 1H-Pyrazole, I believe this compound will play a more active role in future production and life. 288-13-1

Following General Procedure A (90 0C, 30 hours), 1H-pyrazole (205 mg, 3.0 mmol) is coupled with 1-(4-bromophenyl)ethanone (398 mg, 2.0 mmol). The crude brown oil is purified by flash chromatography on silica gel (eluent: dichloromethane/hexanes = 50/50) to provide 300 mg (81 % isolated yield) of the desired product as a white solid. IdentificationMp: 108 JOC.1H NMR (400 MHz, CDCI3): delta 7.98-8.00 (m, 3H, H3|5,7), 7.70-7.76 (m, 3H, H2>6.9), 6.46 (s, 1H, H8), 2.56 (s, 3H, H11).13C NMR (100 MHz, CDCI3): delta 196.84 (C10), 143.33 (C1), 142.09 (C9), 134.80 (C4), 130.01 (C3,beta), 126.91 (C7), 118.39 (C216), 108.62 (C8), 26.60 (C11).IR (KBr) : v (crrf1) = 3135, 3114, 3101 , 1673(C=O), 1605, 1528, 1395, 1264,1210, 935, 838, 762, 611 , 589, 518.GC/MS: rt = 19.96 min, M/Z = 186.HRMS: 187.0893 (M+H). Theoretical: 187.0871.

The chemical industry reduces the impact on the environment during synthesis 288-13-1. I believe this compound will play a more active role in future production and life.

288-13-1, These common heterocyclic compound, 288-13-1, name is 1H-Pyrazole, 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.

Reference Production Example 1-1 1H-pyrazole-1-ylmethanol The mixture of 2.04 g of pyrazole, 2.00 g of paraformaldehyde and 1 ml of triethylamine was stirred at 130 C for 10 hours. After the reaction mixture was cooled to room temperature, acetone was added to the reaction mixture, and then the mixture was filtered. The filterate was concentrated under reduced pressure. Hexane was added to the residue, and then crystalline was formed. The crystalline was collected to obtain 3.10 g of 1H-pyrazole-1-ylmethanol. 1H-NMR(CDCl3,TMS,delta(ppm)):5.51(2H,s),6.30(1H,t),7.58-7.61(2H, m)

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 288-13-1.

288-13-1, The chemical industry reduces the impact on the environment during synthesis 288-13-1, name is 1H-Pyrazole, I believe this compound will play a more active role in future production and life.

General procedure: 1-benzyl-4-chloro-3,5-dimethyl-1H-pyrazole. To a 16 mL vial containing 1-benzyl-3,5-dimethyl-1H-pyrazole (196 mg, 1.05 mmol) and a magnetic stir bar, 0.7 mL of water and 0.3 mL of ethyl acetate was added. Next, NaCl (123 mg, 2 mmol) was added and the vial was placed in a room temperature water bath to control exotherms. Finally, Oxone (322 mg, 0.52 mmol or 1.05 mmol KHSO5) was added and the vial was capped. The reaction proceeded with continuous and vigorous stirring until no starting material remained as indicated by TLC (1 h). The remaining oxidants were reduced with solid sodium bisulfite until starch iodide paper tested negative. Water (5 mL) was added and the mixture was extracted with 1:1 hexanes/diethyl ether (3 x 5 mL). The combined organic fractions were dried (MgSO4) and concentrated to yield crude product that was purified by flash chromatography (14 x 1 cm), 9:1 hexane/ethyl acetate eluent. Pure 1-benzyl-4-chloro-3,5-dimethyl-1H-pyrazole was obtained as a pale yellow oil (215 mg, 93% yield).

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

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

To the suspension of sodium hydride (1.10 eq.) in tetrahydrofurane (0.20 mL/rnmol) wasadded the solution of pyrazole (1.0 eq.) in tetrahydrofurane (0.12 mL/mmol) dropwise,while the temperature was kept under 20 C. After the mixture was stirred at room temperature for 30 minutes, the appropriate halide (1.20 eq.) was added and the mixture was stirred further at same temperature for 16 hours. Next, the reaction mixture was refluxed for 15 hours. After completion the resulting precipitate was filtered off; the filtratewas concentrated then the residue was poured onto a mixture of water and ethyl acetate. The phases were separated, and the aqueous layer was extracted with ethyl acetate. The combined organic layers were dried over Na2SO4, filtered and concentrated under reduced pressure. The crude product was purified via distillation. Using 2-bromopropanc in General Procedure 9G 1-isopropylpyrazole was obtained.

Statistics shows that 1H-Pyrazole is playing an increasingly important role. we look forward to future research findings about 288-13-1.

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.

Pyrazole (16g, 235mmol) was added in portions to sulfuric acid, 98%, (10OmL) keeping the temperature below 4O0C. To this solution was added nitric acid, 70%, (16mL) maintaining the temperature below 550C. After addition the reaction was heated at 550C for 3hours, and then cooled to O0C, before carefully adding to ice / water (40OmL) with stirring. This mixture was neutralized by the careful addition of aqueous 50% sodium hydroxide solution using external cooling and efficient stirring. The resultant solution was extracted with ethyl acetate (3x 30OmL), and the combined extracts were washed with brine (2x250mL) dried (Na2SO4) and concentrated in vacuo to yield a white solid, which was used without further purification, 24.74g, 93%.

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.

288-13-1, A common compound: 288-13-1, name is 1H-Pyrazole, 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.

General procedure: In 50 mL round bottom flask, aryl halide (1.0 mmol), pyrazole (1.2 mmol), ligand (0.04 mmol), Cu2O (0.10 mmol), cesium carbonate (2.0 mmol), and dry solvent (20 mL) were placed under nitrogen atmosphere. The reaction mixture was heated in oil bath up to specified temperature under constant stirring for 20 h and then allowed to cool to room temperature. The reaction mixture was filtered through a plug of Celite in a fritted filter funnel and washed with ethyl acetate. If DMSO is used as solvent, it is extracted by washing the filtrate with 25 mL water for three times. The organic phase was dried over anhydrous MgSO4 and was removed under reduced pressure to provide the crude product which was purified by column chromatography on silica gel, using hexane and ethyl acetate in 3:1 ratio, respectively, as an eluent.

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, 1H-Pyrazole, other downstream synthetic routes, hurry up and to see.

288-13-1, 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 288-13-1 as follows.

EXAMPLE 1; Preparation of 2-Amino-3-methyl-5-(1-methyl-1H-pyrazol-4-yl)-5-(3-pyrimidin-5-ylphenyl)-3,5-dihydro-4-imidazol-4-one; Step a); Preparation of Compound 2; A mixture of pyrazole (3.00 g, 44.0 mmol), iodine (6.71 g, 26.4 mmol) and ceric ammonium nitrate (14.5 g, 26.4 mmol) in acetonitrile (400 mL) was stirred at room temperature for 2.5 h. The reaction was concentrated and partitioned between ethyl acetate (250 mL) and 5% aqueous sodium bisulfite (250 mL). Water (150 mL) was added and the organic layer was separated and washed with brine (250 mL), dried over magnesium sulfate, filtered and concentrated to afford 2 (7.80 g, 91%) as a white solid: mp 105-108 C.; 1H NMR (300 MHz, CDCl3) delta7.63 (s, 2H).

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

These common heterocyclic compound, 288-13-1, name is 1H-Pyrazole, 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. 288-13-1

Pyrazole (8.5 g) and cold concentrated nitric acid (18 cm3, d = 1.4 g/mL) were added to concentrated sulfuric acid (15 cm3) that had been cooled to 0 C using an ice-salt bath.The reaction mixture was heated under reflux for 3 h. The reaction mixture was cooled toroom temperature, and additional nitrating mixture (6 cm3 of concentrated sulfuric acid and 6 cm3 of nitric acid) was added dropwise. The mixture was heated under reflux for a further 3 h, cooled and left to stand overnight. The obtained solution was poured onto ice (80 g), and the precipitate was filtered under reduced pressure, washed with cold water and cold ethanol, and crystallized from toluene. 4-Nitropyrazole (56 % yield) was obtained as a white solid.

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 288-13-1.

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. 288-13-1, name is 1H-Pyrazole, A new synthetic method of this compound is introduced below., 288-13-1

4-nitro-1H-pyrazole Pyrazole (10 g, 147 mmol), was added to concentrated sulfuric acid (100 mL), in portions, while maintaining the internal reaction temperature below 50 C. via an ice water bath. Concentrated nitric acid (10 mL) was then added, dropwise, maintaining the internal reaction temperature below 50 C. via an ice water bath. The ice water bath was removed and the reaction was heated to 60 C. and stirred for 4 hours. The reaction was cooled via an ice water bath and made basic, to ?pH 8, with 18 N aqueous NaOH solution (150 mL). The product, which precipitated as a white solid, was collected by filtration, washed with H2O, and dried under high vacuum to afford 4-nitro-1H-pyrazole (7 g, 42%) as a white solid. 13C NMR (100 MHz, CDCl3): delta 126.4, 137.0.

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.