Category: 10010-93-2

Electric Literature of 10010-93-2, 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 10010-93-2 as follows.

a) A mixture of potassium carbonate (922 mg, 6.67 mmol), 2-methyl-5-(trifluoromethyl)-1H-pyrazole (500 mg, 3.33 mmol) and ethyl 2-bromopropanoate (0.48 mL, 3.7 mmol) in dimethylformamide:tetrahydrofuran (3 mL:6 mL) was heated at 60 C. for 5 h with stirring. After cooling to room temperature, most of tetrahydrofuran was removed by gently blowing nitrogen over the reaction mixture. Ethyl acetate and water were added and the layers were separated. The aqueous layer was extracted twice more with ethyl acetate. The combined organic layers were dried (Na2SO4), filtered, and concentrated in vacuo. The crude residue was purified by flash chromatography (SiO2, 10-20% ethyl acetate in hexanes) to afford the desired product (735 mg, 2.94 mmol, 88%).

According to the analysis of related databases, 10010-93-2, the application of this compound in the production field has become more and more popular.

Synthetic Route of 10010-93-2, A common heterocyclic compound, 10010-93-2, name is 3-Methyl-5-(trifluoromethyl)-1H-pyrazole, molecular formula is C5H5F3N2, 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.

[00143] Step 1: A mixture of 2-chloro-l-(l-(4-chloro-3-methoxyphenyl)piperidin- 4-yl)ethanone (580 mg, 1.919 mmol; see Example Ia, Step 2), 5-methyl-3- (trifluoromethyl)-lH-pyrazole (576 mg, 3.84 mmol), potassium carbonate (796 mg, 5.76 mmol) and acetonitrile (20 mL) was stirred at RT for 12 h. After this time, the solvent was removed under reduced pressure and the resultant residue was partitioned between EtOAc (10OmL) and water (50 mL). The organic phase was washed with brine, dried (TS^SO4) and concentrated on a rotary evaporator to yield a residue. The residue was purified by flash chromatography using a 40 g silica gel cartridge and gradient elution from 10: 1 Hex/EtOAc to 1 : 1 Hex/EtOAc. The fractions containing the product were pooled and concentrated on a rotary evaporator to give l-(l-(4- chloro-3-methoxyphenyl)piperidin-4-yl)-2-(5-methyl-3-(trifluoromethyl)-lH-pyrazol- l-yl)ethanone (650 mg, 1.563 mmol, 81 % yield) as clear oil. 1H-NMR (400 MHz, CDCl3) delta ppm 7.19 (1 H, d, J=8.57 Hz), 6.49 (1 H, d, J=2.42 Hz), 6.44 (1 H, dd, J=8.68, 2.53 Hz), 6.35 (1 H, s), 5.01 – 5.04 (2 H, m), 3.84 – 3.89 (3 H, m), 3.62 – 3.69 (2 H, m), 2.77 (2 H, td, J=12.03, 2.75 Hz), 2.58 (1 H, tt, J=I 1.29, 3.87 Hz), 2.21 (3 H, s), 1.99 (2 H, s), 1.80 – 1.91 (2 H, m).

The synthetic route of 10010-93-2 has been constantly updated, and we look forward to future research findings.

Synthetic Route of 10010-93-2, A common heterocyclic compound, 10010-93-2, name is 3-Methyl-5-(trifluoromethyl)-1H-pyrazole, molecular formula is C5H5F3N2, 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.

[00143] Step 1: A mixture of 2-chloro-l-(l-(4-chloro-3-methoxyphenyl)piperidin- 4-yl)ethanone (580 mg, 1.919 mmol; see Example Ia, Step 2), 5-methyl-3- (trifluoromethyl)-lH-pyrazole (576 mg, 3.84 mmol), potassium carbonate (796 mg, 5.76 mmol) and acetonitrile (20 mL) was stirred at RT for 12 h. After this time, the solvent was removed under reduced pressure and the resultant residue was partitioned between EtOAc (10OmL) and water (50 mL). The organic phase was washed with brine, dried (TS^SO4) and concentrated on a rotary evaporator to yield a residue. The residue was purified by flash chromatography using a 40 g silica gel cartridge and gradient elution from 10: 1 Hex/EtOAc to 1 : 1 Hex/EtOAc. The fractions containing the product were pooled and concentrated on a rotary evaporator to give l-(l-(4- chloro-3-methoxyphenyl)piperidin-4-yl)-2-(5-methyl-3-(trifluoromethyl)-lH-pyrazol- l-yl)ethanone (650 mg, 1.563 mmol, 81 % yield) as clear oil. 1H-NMR (400 MHz, CDCl3) delta ppm 7.19 (1 H, d, J=8.57 Hz), 6.49 (1 H, d, J=2.42 Hz), 6.44 (1 H, dd, J=8.68, 2.53 Hz), 6.35 (1 H, s), 5.01 – 5.04 (2 H, m), 3.84 – 3.89 (3 H, m), 3.62 – 3.69 (2 H, m), 2.77 (2 H, td, J=12.03, 2.75 Hz), 2.58 (1 H, tt, J=I 1.29, 3.87 Hz), 2.21 (3 H, s), 1.99 (2 H, s), 1.80 – 1.91 (2 H, m).

The synthetic route of 10010-93-2 has been constantly updated, and we look forward to future research findings.

10010-93-2, name is 3-Methyl-5-(trifluoromethyl)-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. Quality Control of 3-Methyl-5-(trifluoromethyl)-1H-pyrazole

An oven dried resealable Schlenk tube was charged with 5-bromopyridin-2-amine (400 mg, 2.24 mmol), 5-methyl-3-(trifluoromethyl)-1H-pyrazole (340 mg, 2.24 mmol), potassium phosphate (972 mg, 4.49 mmol) and 7 ml dioxane were added. The Schlenk tube was subjected to three cycles of evacuation-backfilling with argon, and copper(I) iodide (65 mg, 0.34 mmol) and N,N’-dimethylcyclohexane-1,2-diamine (55 mul, 0.34 mmol) were added. After three further cycles of evacuation-backfilling with argon, the Schlenk tube was capped and placed in an oil bath at 130 C overnight. The mixture was cooled and was filtered through a plug of Celite. The filtered was concentrated under reduced pressure and the brown crude was purified by flash chromatography (0% to 50%, hexane-ethyl acetate) to give 476 mg (88% yield) of the title compound. LRMS (m/z): 343 (M+1)+.

The synthetic route of 10010-93-2 has been constantly updated, and we look forward to future research findings.

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. 10010-93-2, name is 3-Methyl-5-(trifluoromethyl)-1H-pyrazole belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below. SDS of cas: 10010-93-2

Example 8 Synthesis of 1-[1-(4-fluorophenyl)-6,7-dihydro-5H-pyrazolo[4,3-b]pyridin-4-yl]-2-[5-methyl-3-(trifluoromethyl)pyrazol-1-yl]ethanone 2-Chloro-1-(1-(4-fluorophenyl)-6,7-dihydro-1H-pyrazolo[4,3-b]pyridin-4(5H)-yl)ethanone (118 mg, 0.4 mmol) was diluted in 1.2 mL of 2:1 THF:DMF and treated with K2CO3 (111 mg, 0.8 mmol) and 5-methyl-3-(trifluoromethyl)-1H-pyrazole (60 mg, 0.4 mmol). The slurry was heated to 75 C. for 2 hours. The reaction slurry was purified by normal phase flash chromatography (24 g column, eluting with 10-80% EtOAc in hexanes) to provide 109 mg (67%) of the title compound as a white solid. 1H NMR (400 MHz, CDCl3) delta 8.36 (s, 0.8H), 7.59 (s, 0.2H), 7.42-7.47 (m, 2H), 7.12-7.25 (m, 2H), 5.25 (s, 0.4H), 5.14 (s, 1.6H), 3.92 (m, 0.4H), 3.86 (m, 1.6H), 2.86 (t, J=6.2 Hz, 2H), 2.37 (s, 2.4H), 2.36 (m, 0.6H), 2.11 (m, 1.6H), 2.04 (m, 0.4H); MS: (ES) m/z calculated for C19H18F4N5O [M+H]+ 408.1, found 408.1.

The synthetic route of 10010-93-2 has been constantly updated, and we look forward to future research findings.

Some common heterocyclic compound, 10010-93-2, name is 3-Methyl-5-(trifluoromethyl)-1H-pyrazole, molecular formula is C5H5F3N2, 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. 10010-93-2

Dissolve 5-methyl-3-(trifluoromethyl)pyrazole (1.00 g, 6.66 mmol) in 60% aqueous acetic acid (13 mL). Add sodium acetate (0.819 g, 9.99 mmol) and cool to 0 0C. Add bromine (1.17 g, 7.33 mmol) dropwise over 10 min.. Stir at 0 0C for 3 hr, then at room temperature for 18 hr. Add ethyl acetate and saturated aqueous sodium sulfite solution. Separate organics and wash one time with saturated aqueous sodium bicarbonate solution followed by saturated aqueous sodium chloride. Dry (magnesium sulfate), filter and concentrate to give 4-bromo-5-methyl-3-trifluoromethyl-lH-pyrazole (1.50 g, 100%). GC-MS: m/z = 229 [M+].

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 10010-93-2, its application will become more common.

10010-93-2, 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. 10010-93-2 name is 3-Methyl-5-(trifluoromethyl)-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.

a) A mixture of potassium carbonate (924 mg, 6.69 mmol), 2-methyl-5-(trifluoromethyl)-1H-pyrazole (501 mg, 3.34 mmol) and methyl 2-bromobutyrate (0.42 mL, 3.7 mmol) in dimethylformamide:tetrahydrofuran (3 mL:6 mL) was heated at 60 C. for 5 h with stirring. After cooling to room temperature, most of tetrahydrofuran was removed by gently blowing nitrogen over the reaction mixture. Ethyl acetate and water were added and the layers were separated. The aqueous layer was extracted twice more with ethyl acetate. The combined organic layers were dried (Na2SO4), filtered, and concentrated in vacuo. The crude residue was purified by flash chromatography (SiO2, 12-17% ethyl acetate in hexanes) to afford the desired product (704 mg, 2.81 mmol, 84%).

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