Day: February 22, 2021

Reference of 345637-71-0,Some common heterocyclic compound, 345637-71-0, name is 2-(5-Methyl-3-(trifluoromethyl)-1H-pyrazol-1-yl)acetic acid, molecular formula is C7H7F3N2O2, 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 room temperature, a solution of trifluoroacetic acid solution (30% in dichloromethane, 2 ml) is added dropwise to tert-butyl 4-{4-[(1-naphthylsulphanyl)methyl]-1,3-thiazol-2-yl}piperidine-1-carboxylate (269 mg). The reaction mixture is stirred for 30 minutes, and triethylamine (2 ml) is then added to the reaction mixture.Oxalyl chloride (232 mg) and a drop of N,N-dimethylformamide are added to a solution of [5-methyl-3-(trifluoromethyl)-1H-pyrazol-1-yl]acetic acid (140 mg) in dichloromethane (5 ml). The reaction mixture is then stirred for 30 minutes. Excess oxalyl chloride is then removed under reduced pressure, and the residue is re-dissolved in dichloromethane (1 ml). The solution is then added to the first solution of trifluoroacetic acid 4-{4-[(1-naphthylsulphanyl)methyl]-1,3-thiazol-2-yl}piperidine (1:1) (III-1) in dichloromethane and triethylamine. The reaction mixture is then warmed to room temperature and stirred for another 20 hours. The solvent is then removed under reduced pressure. The residue is purified by column chromatography. This gives 2-[5-methyl-3-(trifluoromethyl)-1H-pyrazol-1-yl]-1-(4-{4-[(1-naphthylsulphanyl)methyl]-1,3-thiazol-2-yl}piperidin-1-yl)ethanone (134 mg, 36%).logP (pH2.7): 4.331H NMR (CD3CN, 400 MHz): deltappm: 1.50-1.80 (m, 2H), 2.15-2.25 (m, 2H), 2.23 (s, 3H), 2.90 (bs, 1H), 3.20 (m, 1H), 3.25 (bs, 1H), 3.90 (bs, 1H), 4.25 (s, 2H), 4.38 (bs, 1H), 5.04 (bs, 2H), 6.37 (s, 1H), 6.87 (s, 1H), 7.41 (dd, 1H), 7.48-7.56 (m, 2H), 7.63 (d, 1H), 7.80 (d, 1H), 7.89 (m, 1H), 8.33 (s, 1H)MS (ESI): 531 ([M+H]+)

The synthetic route of 345637-71-0 has been constantly updated, and we look forward to future research findings.

Adding a certain compound to certain chemical reactions, such as: 930-36-9, name is 1-Methylpyrazole, 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 930-36-9, Product Details of 930-36-9

S1, under nitrogen atmosphere protection,100g of 1-methylpyrazole was added to 2L of tetrahydrofuran, stirred to dissolve to uniform state,Then cooled to minus 60 degrees,Then 2.5M concentration of n-butyllithium 600ml,Insulation below minus 60 degrees Celsius,After the addition of n-butyl lithium is completed, and then incubated 0.4h,Cooled to minus 65 degrees Celsius,100 mL of N, N-dimethylformamide was added dropwise,After dropping N, N-dimethylformamide overnight at room temperature,The whole was cooled to 0 degrees Celsius, 300ml deionized water was added dropwise after quenching.S2, extracted with 500 ml of ethyl acetate each time,Repeat 2 times to separate the organic phase,Each time with 500ml saturated brine wash,Repeat washing 2 times, with 50g anhydrous sodium sulfate drying 1h,Suction filtration, then decompression rotary steaming,The product from S2 step is 1-methyl-1H-pyrazole-5-carbaldehyde.

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

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. 26621-44-3, name is 3-Nitro-1H-pyrazole belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below. Safety of 3-Nitro-1H-pyrazole

The 2-(4-hydroxy-but-2-ynyl)-isoindole-1,3-dione (1.29 g, 6.00 mmol), 3-Nitro-1H-pyrazole (prepared in example 3, 655 mg, 5.80 mmol) and triphenylphosphine (1.57 g, 6.00 mmol) were combined and dissolved in tetrahydrofuran (30 mL) and then chilled to 0 C. While stirring, diisopropyl azodicarboxylate (1.77 mL, 9 mmol) was added dropwise. The ice bath was removed and the reaction continued to stir at 25 C. for 1 h. At this point the desired product had precipitated. Collection of the precipitate using in vacuo filtration followed by rinsing with tetrahydrofuran (2¡Á10 mL) then drying in vacuo for 2 h afforded 2-[4-(3-nitro-pyrazol-1-yl)-but-2-ynyl]-isoindole-1,3-dione (1.54 g, 86%) as a white powder: ESI-LRMS m/e calcd for C15H10N4O4 [M+] 310.07, found 311.17 [M+H+], 621.20 [2M+H+].

The synthetic route of 26621-44-3 has been constantly updated, and we look forward to future research findings.

Application of 120068-79-3,Some common heterocyclic compound, 120068-79-3, name is 5-Amino-1-(2,6-dichloro-4-(trifluoromethyl)phenyl)-1H-pyrazole-3-carbonitrile, molecular formula is C11H5Cl2F3N4, 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.

Further comparative experiments are conducted employing the following preparation procedure; To a 750 ml reactor with a mechanical stirrer and a thermometer containing the amine acid complex (1.5 eq.), 147 g anhydrous toluene (6.5 eq.), and 44.8 g CF3SOCI (1.2 eq.) under an argon atmosphere at 0 0C was added vacuum dried 5-amino-1-(2,6- dichloro-4-trifluoromethyl-phenyl)-1 H-pyrazole-3-carbonitrile (1 eq., 79.5 g, 245 mmol, 99 % purity). The reaction mixture was kept at 5 0C for 60 min and then heated to 35 0C within 45 min. The temperature of 35 0C was kept for another 10 hours before quenching the reaction with 200 g of sodium hydroxide solution (10 wt.%). The resulting suspension was diluted with 176 ml of ethylacetate. After phase separation the organic layer was washed once with sodium hydroxide solution (10 wt.%). After phase separation, the organic layer was analyzed by quantitative HPLC. The product was crystallized from a mixture of ethylacetate and toluene affording the title compound as a white crystalline powder.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 5-Amino-1-(2,6-dichloro-4-(trifluoromethyl)phenyl)-1H-pyrazole-3-carbonitrile, its application will become more common.

Synthetic Route of 1128-54-7,Some common heterocyclic compound, 1128-54-7, name is 3-Methyl-1-phenyl-1H-pyrazole, molecular formula is C10H10N2, 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.

General procedure: A clean and oven dry sealed tube was charged with 1-phenylpyrazole (1equiv.), and styrene (2.5equiv.), to this added (Rh-Complex 0.5mol%) and Cu(OAc)2.H2O (1 equiv), of water (1mL) as a reaction medium. Thereafter, the reaction mixture was heated at 90-100C under sealed conditions for 12h. The gain in product formation was examined by periodic monitoring through TLC. Then the reaction mixture was cool to room temperature, added water (50mL) and EtOAc (75mL) and the organic layer was extracted thrice, and dried over the anhydrous Na2SO4. The crude product was obtained by evaporating the solvent under reduced pressure. Finally, the product was purified through column chromatography (EtOAc/hexane).

The synthetic route of 1128-54-7 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. 1192-21-8, name is 1-Methyl-1H-pyrazol-5-amine, A new synthetic method of this compound is introduced below., Quality Control of 1-Methyl-1H-pyrazol-5-amine

Example 1.26; Preparation of (4′-Fluoro-biphenyl-4-yI)-(2-methyl-2Eta-pyrazol-3-yl)-amine (Compound35). A 20-mL scintillation vial was charged with 4′-bromo-4-fluoro-biphenyl (251.1 mg, 1 mmol), 3 -amino-2 -methyl pyrazole (97.1 mg, 1 mmol), sodium terf-butoxide (134.5 mg, 1.4 , mmol), tris(dibenzylideneacetone)dipalladium(0) (45.8 mg, 0.05 mmol), BINuAP (62.3 mg, 0.1 mmol) and toluene (2 mL) under nitrogen atmosphere. The reaction mixture was heated at 800C for 48 hours. It was then allowed to cool to room temperature, taken up in ether/ethyl acetate, filtered and concentrated. The crude material was subjected to column chromatography on silica gel (Biotage, eluent hexanes/ethyl acetate 70/30) to afford Compound 35 as a yellow solid. LCMS m/z (percent) = 268 (M+H, 100).

The synthetic route of 1192-21-8 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. 151049-87-5, name is 3-Bromo-1-methyl-1H-pyrazole, A new synthetic method of this compound is introduced below., Application In Synthesis of 3-Bromo-1-methyl-1H-pyrazole

To a mixture of 8-3 (80 mg, 0.21 mmol, 1.0 eq) and 8-3a (44 mg, 0.27 mmol, 1.3 eq) in dioxane (3 mL) and H20 (0.15 mL) was added Na2CC>3 (44 mg, 0.42 mmol, 2.0 eq) and Pd(dppf)Cl2 (16 mg, 21 umol, 0.1 eq) in one portion under N2. The mixture was stirred at 100 C for 16 h. LCMS showed the starting material was consumed completely and one peak with desired MS was detected. The reaction mixture was concentrated under reduced pressure to remove solvent, and then added CH3CN (5 mL), filtered to give a black-brown liquid. The residue was purified by prep-HPLC. LCMS and XH NMR confirmed that Compound 8 was obtained (2.20 mg, 6.4 umol, 3.0% yield). LCMS (ESI): RT = 0.835 min, mass calcd. For C17H23N3O2S, 333.15 m/z found 333.9[M+H]+ 1H NMR (400MHz, CDC13) delta 8.44 (br d, J= 7.20 Hz, 1H), 8.04 (s, 1H), 7.64 (br d, J= 8.00 Hz, 1H), 7.41 (br s, 1H), 6.76 (br d, J= 8.80 Hz, 1H), 6.68 (s, 1H), 3.96 (s, 3H), 3.54 (br s, 1H), 3.04 (s, 3H), 2.10 – 2.00 (m, 2H), 1.87 – 1.75 (m, 2H), 1.68 – 1.55 (m, 2H), 1.50 – 1.42 (m, 3H).

The synthetic route of 151049-87-5 has been constantly updated, and we look forward to future research findings.

Adding a certain compound to certain chemical reactions, such as: 3994-50-1, name is 1-Methyl-4-nitro-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 3994-50-1, Recommanded Product: 1-Methyl-4-nitro-1H-pyrazole

A mixture of a portion (0.7 g) of the material so obtained, platinum oxide (0.05 g), ethyl acetate (5 ml) and ethanol (15 ml) was stirred under 3 atmospheres pressure of hydrogen for 2 hours. The catalyst was removed by filtration and the filtrate was evaporated. There was thus obtained the required starting material (0.6 g); 1H NMR: (DMSOd6) 3.64 (s, 3H), 6.86 (s, IH), 6.97 (s, IH).

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.

Reference of 35277-02-2, 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. 35277-02-2, name is 4-Fluoro-1H-pyrazole belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

To 4-fluoro-lH-pyrazole, 28-d, (2g, 23mmol) and cyanamide (0.97g, 23mmol) in dioxane (5mL) was added 4N HC1 in dioxane (15mL). The mixture was gently refluxed with stirring for 2h under nitrogen. During the course of the reaction the product crystallizes. After cooling to room temperature, 10 mL of anhydrous ether was added and the mixture was allowed to stand for 30min. The white solid was collected by filtration, washed with anhydrous ether and dried to constant weight in vacuuo providing the product, 28-e, (3g, 80%)

The synthetic route of 4-Fluoro-1H-pyrazole has been constantly updated, and we look forward to future research findings.

Application of 304903-10-4, These common heterocyclic compound, 304903-10-4, name is 1-Ethyl-1H-pyrazole-4-carbaldehyde, 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.

A mixture of 1-ethylpyrazole-4-carbaldehyde [0.322 g (2.6 mmol)], malonic acid [0.530 g (5.2 mmol)], pyridine (5 mL) and piperidine (0.050 mL) was stirred at 80 C. for 1 h followed by stirring for 3 h at 115 C. The reaction was then poured into water (100 mL) and acidified with conc. HCl. The resulting white ppt., product, was filtered and vacuum dried. Yield=436 mg (99%) MS (m/z): 169 [M+H]

Statistics shows that 1-Ethyl-1H-pyrazole-4-carbaldehyde is playing an increasingly important role. we look forward to future research findings about 304903-10-4.