Category: 2458-26-6

2458-26-6, name is 3-Phenyl-1H-pyrazole, 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. Formula: C9H8N2

General procedure: A mixture of acetophenone and dimethylformamide dimethylacetal (2.0 equiv.) was refluxed overnight. The reaction mixture was allowed to cool down to room temperature and was concentrated under reduced pressure. The remaining residue was suspended in hexanes and filtered. The filter cake was washed with plenty of hexanes. (E)- 3-(dimethylamino)-l- phenylprop-2-en-l-one was obtained. (0260) Hydrazine-monohydrate (5.0 equiv.) was added to a solution of (E)- 3- (dimethylamino)-l-phenylprop-2-en-l-one in EtOH and the resulting reaction mixture was refluxed for 2 hours. The reaction was then allowed to cool down to room temperature and was concentrated under reduced pressure. The remaining residue was diluted with H2O and extracted with CH2CI2. The organic phase was dried over MgS04, filtered and concentrated under reduced pressure. The residue was considered pure enough by -NuMuKappa (>95%) to be used without further purification. (0261) A mixture of phenylpyrazole, iodoarene (1.0 equiv.), copper iodide (20 mol%), trans- (0262) 1,2-diaminocyclohexane (25 mol%), potassium carbonate (2.0 equiv.) in dioxane was stirred at 100C under argon for 16 hours. After cooling down to room temperature, the reaction mixture was diluted with H2O and extracted with EtOAC. The gathered organic phases were washed with NH4CI/NH3 (v/v : 1/1), brine, dried over MgSC , filtered and concentrated under reduced pressure. The remaining residue was purified by column chromatography on silica gel (Hexanes/EtOAc).

The synthetic route of 2458-26-6 has been constantly updated, and we look forward to future research findings.

Related Products of 2458-26-6, 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. 2458-26-6, name is 3-Phenyl-1H-pyrazole, This compound has unique chemical properties. The synthetic route is as follows.

To a solution of ethyl2-chloronicotinate (2 g, 10.78 mmol) and 3-phenyl-1H-pyrazo1e (2.33 g, 16.16 mmol) in DMF (30 mL) was added K2C03 (4.47 g, 32.33 mmol)and Kl (1.79 g, 10.78 mmol). The mixture was stirred at 130 oc for 16h. The reaction wasfiltered, the filtrate was added I-hO (100 mL), extracted with EA (30 mL x2), the organicphase was washed with brine ( l 00 mL ), filtered, and concentrated. The residue was purifiedby flash silica gel chromatography (ISCO; 40 g SepaFlash Silica Flash Column, Eluent of15(% Ethyl acetate/Petroleum ethergradient 40 mUmin). Compound 113A (1 g, yield:28.5%) was obtained as a white solid. 1H NMR (400MHz, CDCh) 8 8.49 (dd, J = 1.7, 4.6Hz, lH), 8.42 (d, J”‘ 2.4 Hz, 1H), 7.94 (dd, J ‘” 1.7, 7.6 Hz, lH), 7.89- 7.78 (m, 2H), 7.40 (t,J “‘ 7.3 Hz, 2H), 7.33 (br d, J ‘” 7.3 Hz, H-I), 7.29 – 7.23 (m, HI), 6.79 (d, J “‘ 2.7 Hz, HI),4.45- 4.25 (m, 2H), 1.14 (t, J = 7.2 Hz, 3H). MS (ESl) m/z (M+Ht294.1.

The chemical industry reduces the impact on the environment during synthesis 3-Phenyl-1H-pyrazole. I believe this compound will play a more active role in future production and life.

Application of 2458-26-6,Some common heterocyclic compound, 2458-26-6, name is 3-Phenyl-1H-pyrazole, molecular formula is C9H8N2, 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.

At 0 C, a solution of 3-phenyl-1H-pyrazole (0.61 g, 5.3 mmol) in dry THF (10 mL) was added dropwise to a suspension of NaH (0.13 g,5.34 mmol) in dry THF (10 mL). After 15 min of stirring, a solution of 2,6-pyridine-dimethylene-ditosylate (1.20 g, 2.67 mmol) in dry THF (15 mL) was added to this solution; the mixture was stirred overnight and filtered, and the solvent was removed. The crude product was purified by column chromatography on silica gel with hexane:EA = 1:1 as eluent to afford 0.41 g (40%) of pure ligand as a white oil that solidified with time. Single crystals were obtained by slow diffusion of hexane into a concentrated solution of the ligand in THF at room temperature. 1H NMR (300 MHz, acetone-d6): 7.84(m, 2H, 4H, 5-H Pz, 2,6-H Ph), 7.65 (t, J = 7.8 Hz, 1H, 4-H Py), 7.36(t, J = 7.2 Hz, 4H, 3,5-H Ph), 7.26 (t, J = 7.5 Hz, 2H, 4-H Ph), 6.96 (d,J = 7.8 Hz, 2H, 3,5-H Py), 6.72 (d, J = 2.4 Hz, 2H, 4-H Pz), and 5.48 (s,4H, PyCH2Pz).13C NMR (75 MHz, acetone-d6): 157.9 (2C, 2,6-CPy), 152.2 (2C, 3-C Pz), 138.9 (1C, 4-C Py), 134.8 (2C, 1-C Ph), 132.9(2C, 5-C Pz), 129.3(4C, 3,5-C Ph), 128.2 (2C, 4-C Ph), 126.1 (4C, 2,6-CPh), 121.2 (2C, 3,5-C Py), 103.7 (2C, 4-C Pz), and 57.9 (2C, PyCH2Pz).

The synthetic route of 2458-26-6 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 2458-26-6 as follows. Formula: C9H8N2

Aromatic substrate 1b (0.1mmol), 3-phenylpyrazole 2m (0.15mmol), cuprous bromide (0.1mmol), potassium acetate (0.2mmol), DMSO (1.0mL) were added to the 15mL Schlenk tube, then directly sealed tube at 85 C for 12h. After the reaction was completed, the mixture was cooled to room temperature, and a small amount of ethyl acetate and ammonia were added to quench the reaction. The ethyl acetate was repeatedly extracted. The organic layers were combined, washed with saturated brine, dried over anhydrous sodium sulfate, filtered under reduced pressure, and the solvent was evaporated under reduced pressure. The crude product was separated and purified by a preparative plate (DCM: MeOH = 35: 1) to obtain 3bm as a white solid, 29.4 mg, with a yield of 70%.

According to the analysis of related databases, 2458-26-6, the application of this compound in the production field has become more and more popular.

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. 2458-26-6, name is 3-Phenyl-1H-pyrazole belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below. Safety of 3-Phenyl-1H-pyrazole

General procedure: A solution was prepared from the amine (0.781 mmol) in DCM (5.5 mL) and the boronic acid(1.25 mmol) and NEt3 (0.039 g, 54 muL, 0.391 mmol) were added. A second solution was prepared with Cu(OAc)2*H2O (0.195 mmol, 0.25 equiv), NEt3 (0.039 g, 54 muL, 0.391 mmol) and pyridine (0.062 g, 63 muL, 0.781 mmol) in DCM (5.5 mL). The two solutions were introduced to independent 5 mL sample loop as shown in (Scheme 1). The dispensing HPLC pumps were each set at 0.125 mL/min to achieve a residence time of 2 h. Two reverse ?tubein-tube? reactors were used in series to achieve a combined reactor volume of 30 mL which were heated at 40 C. The reaction mixture was then passed through an Omnifit column (r =0.33 cm, h = 10.00 cm) filled with QP-DMA followed by a back pressure regulator (175 psi).The crude reaction mixture was passed through a plug of silica to remove base line residue and the solvent evaporated under reduced pressure. The resultant crude material was then purified using flash chromatography.

The synthetic route of 2458-26-6 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. 2458-26-6, name is 3-Phenyl-1H-pyrazole, A new synthetic method of this compound is introduced below., HPLC of Formula: C9H8N2

1.57 g of 3-phenylpyrazole was dissolved in 11 ml of N,N-dimethylformamide. To the resulting solution was added 0.50 g of 60% sodium hydride, and the entire mixture was stirred for 1.5 hours at room temperature. To this mixture was added a solution containing 2.90 g of the 1-tert-butoxycarbonylpiperidin-4-yl methanesulfonate dissolved in 2 ml of N,N-dimethylformamide, and the entire mixture was stirred for two hours at 50C, one hour at 70C, and then 3.5 hours at 100C. The reaction liquid was then poured into water, and extracted twice with ether. The organic layer was washed three times with water and dried over anhydrous magnesium sulfate, and the solvent was then removed by evaporation under reduced pressure. The residue was purified by silica gel column chromatography (developing solvent: hexane/ethyl acetate = 4/1 (volume ratio)), yielding 1.54 g of the target compound.

The synthetic route of 2458-26-6 has been constantly updated, and we look forward to future research findings.

Adding some certain compound to certain chemical reactions, such as: 2458-26-6, name is 3-Phenyl-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 2458-26-6. 2458-26-6

Teri-butyl (R )-(2-(3-phenyl-1H-pyrazol- 1 -yl)propyl)carbamate 3-Phenyl-1 H-pyrazole (250 mg, 1 .73 mmol), cesium carbonate (5.65 g, 17.30 mmol) and (S)-1 -((ieri-butoxycarbonyl)amino)propan-2-yl methanesulfonate (876 mg, 3.46 mmol) were combined in anhydrous N,N- dimethylformamide (10 ml). The resulting suspension was heated to 50 C and the progress of the reaction was monitored by TLC. Once the reaction was complete (~ 18 h) the reaction mixture was quenched by addition of water and the product was extracted with ethyl acetate three times. The organic layers were combined and washed with a saturated aqueous solution of sodium chloride. All of the volatiles were removed in vacuo. The crude material was purified by column chromatography, eluting 5-10% ethyl acetate/petroleum spirits to give the title compound as a colourless solid (60 mg, 12%). LRMS [M+H]+ 302.2 m/z; HRMS [M+H]+ 302.1863 m/z, found 302.1867 m/z; 1 H NMR (400 MHz, CDCI3) delta 7.85 – 7.72 (m, 2H), 7.41 – 7.33 (m, 3H), 7.31 – 7.25 (m, 1 H), 6.54 (d, J = 2.3 Hz, 1 H), 5.05 (d, J = 1 .1 Hz, 1 H), 4.26 (dd, J = 13.8, 4.5 Hz, 1 H), 4.21 – 4.10 (m, 1 H), 4.05 (dd, J= 12.6, 6.7 Hz, 1 H), 1 .41 (s, 9H), 1 .12 (d, J = 6.8 Hz, 3H).

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 3-Phenyl-1H-pyrazole.

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. 2458-26-6, name is 3-Phenyl-1H-pyrazole, A new synthetic method of this compound is introduced below., 2458-26-6

3-Phenylpyrazole (2.00 g, 13.87 mmol) as a solid was added to a stirred slurry of NaH (0.33 g, 13.87 mmol) in THF (60 mL) at r.t. After 30 min SOCl2 (0.50 mL, 0.83 g, 6.94 mmol) was added in one portion via syringe and the resulting mixture stirred at r.t. for 5 min. After addition of 3,4-dihydroxybenzaldehyde (0.96 g, 6.94 mmol) and pyridine (5.60 mL, 4.78 g, 60.40 mmol), the reaction mixture was kept at reflux temperature for 16 h. H2O (50 mL) was added and the aqueous phase extracted into CH2Cl2 (3 ¡Á 50 mL). The combined organic extracts were washed with brine, dried over MgSO4, filtered, and the filtrate was evaporated to dryness in vacuo. The crude product was purified by column chromatography (silica gel; CHCl3/EtOAc 1:1). All product-containing fractions were concentrated by rotary evaporation at 40 C and upon cooling to r.t. colorless 1(Ph) precipitated, which was isolated by filtration and washed with Et2O. Yield: 1.53 g (54%). Rf = 0.63 (silica gel, CHCl3/EtOAc 1:1). 1H NMR (400.1 MHz, d6-DMSO) delta = 6.48 (dd, 3JHH = 8.3, 4JHH = 2.0, 1 H; HQ-H6), 6.66 (d, 4JHH = 2.0, 1 H; HQ-H2), 6.76 (d, 3JHH = 8.3, 1 H; HQ-H5), 6.84 (d, 3JHH = 2.5, 2 H; pz-H4), 7.31 (m, 2 H; Ph-H4), 7.41 (m, 4 H; Ph-H3), 7.82 (m, 4 H; Ph-H2), 7.91 (s, 1 H; CH), 7.94 (d, 3JHH = 2.5, 2 H; pz-H5), 9.15 (bs, 2 H; OH). 13C NMR (100.6 MHz, d6-DMSO) delta = 76.7 (Cpz2), 103.5 (pz-C4), 114.4 (HQ-C2), 115.5 (HQ-C5), 118.2 (HQ-C6), 125.3 (Ph-C2), 127.2 (HQ-C1), 127.8 (Ph-C4), 128.7 (Ph-C3), 131.9 (pz-C5), 132.8 (Ph-C1), 145.3, 146.1 (HQ-C3,4), 151.0 (pz-C3). ESI-MS: m/z (%) 263 (67) [M – Phpz]-, 408 (100) [M – H]-. Anal. Calcd (%) for C25H20N4O2 (408.45): C 73.51, H 4.94, N 13.72. Found: C 73.22, H 4.86, N 13.67.

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.

The chemical industry reduces the impact on the environment during synthesis 2458-26-6, name is 3-Phenyl-1H-pyrazole, I believe this compound will play a more active role in future production and life. 2458-26-6

A solution of 3-phenyl-leta-pyrazole (2.98 g, 20.67 mmol) in anhydrous N,N- dimethylformamide (40 ml) was treated with N-bromosuccinimide (3.68 g, 20.67 mmol) in one portion and then stirred at room temperature for 1 h. The reaction was evaporated under reduced pressure and the resulting residue was dissolved in ethanol (15 ml) and diluted with water (100 ml) to precipitate the crude product. The solids were collected by filtration and dried via air suction. The product was purified by recrystallization from acetonitrile- water to give the title compound (4.19 g, 91 %) as a white solid. MS(ES)+ m/e 224 [M+H]+.

The chemical industry reduces the impact on the environment during synthesis 2458-26-6. I believe this compound will play a more active role in future production and life.

The chemical industry reduces the impact on the environment during synthesis 2458-26-6, name is 3-Phenyl-1H-pyrazole, I believe this compound will play a more active role in future production and life. 2458-26-6

A solution of 3-phenyl-leta-pyrazole (2.98 g, 20.67 mmol) in anhydrous N,N- dimethylformamide (40 ml) was treated with N-bromosuccinimide (3.68 g, 20.67 mmol) in one portion and then stirred at room temperature for 1 h. The reaction was evaporated under reduced pressure and the resulting residue was dissolved in ethanol (15 ml) and diluted with water (100 ml) to precipitate the crude product. The solids were collected by filtration and dried via air suction. The product was purified by recrystallization from acetonitrile- water to give the title compound (4.19 g, 91 %) as a white solid. MS(ES)+ m/e 224 [M+H]+.

The chemical industry reduces the impact on the environment during synthesis 2458-26-6. I believe this compound will play a more active role in future production and life.