Tag: M.W=0-100

Adding a certain compound to certain chemical reactions, such as: 1192-21-8, name is 1-Methyl-1H-pyrazol-5-amine, 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 1192-21-8, Safety of 1-Methyl-1H-pyrazol-5-amine

Degas a mixture of 2-(2-chloropyrimidin-4-yl)-6,6-dimethyl-5-(2- morpholinoethyl)thieno[2,3-c]pyrrol-4-one (20.8 g, 52.9 mmol), 2-methylpyrazol-3-amine (5.7 g, 58.2 mmol), cesium carbonate (37.9 g, 116.5 mmol), 4,5- bis(diphenylphosphino)-9,9-dimethylxanthene (2.6 g, 4.5 mmol) and 1,4-dioxane (529 mL) with nitrogen for 10 minutes. Add tris(dibenzylideneacetone)dipalladium(0) (2.4 g, 2.6 mmol) and heat the mixture to 85 C for four hours. Cool the mixture to room temperature and filter the mixture through filter paper. Concentrate the filtrate under reduced pressure. Repeat the reaction starting with 8 g of 2-(2-chloropyrimidin-4-yl)-6,6- dimethyl-5-(2-morpholinoethyl)thieno[2,3-c]pyrrol-4-one and combine the two residues. Purify the residue by silica gel column chromatography (330 g) eluting with a gradient from 5-25% MeOH in (10% EtOAc in DCM). Pool the fractions and concentrate under reduced pressure. Re-purify the residue by silica gel column chromatography (330 g) eluting with a gradient from 5-25% MeOH in 10% EtOAc in DCM. Pool the fractions and concentrate under reduced pressure. Dissolve the residue in DCM (400 mL) and then add acetone (1 L). Slowly concentrate the mixture under reduced pressure to approximately 700 mL. Collect the solid by vacuum filtration to give the title compound 14.8 g (48%). MS (m/z): 454 (M+1).

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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. 1453-58-3, name is 3-Methylpyrazole belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below. Formula: C4H6N2

Potassium /-butoxide (3.9 g, 0.33 mmol) was dissolved in DMSO (25 mL). To this solution was added 3 -methyl pyrazole (2.7 g, 0.33 mmol) and the reaction was heated at 50 C for 30 min. l-Bromo-4-chloro-2-fluorobenzene (4.6 g, 0.22 mmol) was then added and the reaction was stirred at 50 C for 16 h. The reaction was cooled to RT and extracted with water and EtOAc, washed with brine, and dried over Na2S04) filtered and concentrated in vacuo. Purification by normal phase silica gel column chromatography (EtO Ac/heptane) provided l-(2- bromo-5-chlorophenyl)-3-methyl-lH-pyrazole and l-(2-bromo-5-chloroplienyl)-5-methyl-lH- pyrazole as a 4: 1 mixture that was used in the next step directly,The mixture from Step 1 (8 g, 0.39 mmol) was dissolved in 160 mL of THF and cooled to 0 C. /-Propyl magnesium chloride (2.0 M in THF, 23 mL) was added dropwise and the reaction stirred for 45 min, then ethyl trifluoroacetate (6 mL) was added. The reaction was stirred for 30 min at 0 C, then 10% HC1 was added dropwise (40 mL). The reaction was extracted with water and EtOAc, washed with brine, and dried over Na2S04, filtered, and concentrated in vacuo. Purification by normal phase silica gel column chromatography (EtOAc/heptane) provided l -(4- chloiO-2-(3-methyi-lH-pyrazol-l-yl)phenyl)-2,2,2-trifluoroethanone as a white solid.

The synthetic route of 1453-58-3 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 31230-17-8 as follows. SDS of cas: 31230-17-8

A mixture of 2,4-dichloropyrimidine (0.967 g, 6.49 mmol), 3-amino-5-methylpyrazole (0.63 g, 6.40 mmol), and ethyldiisopropylamine (2.8 mL, 16.22 mmol) in ethanol (13 mL) was stirred at -10C for 2 h, then at r.t. overnight, and finally at 50C for 3.5 h. The mixture was concentrated to a total volume of approximately 10 mL. Upon repeated addition of diethylether, (2-chloropyrimidin-4-yl)-(5-methylpyrazol-3-yl)amine (0.258 g, 1.23 mmol, 19 %) was obtained as colourless crystals. LC/ESI-MS: m/z = 210 [M(35Cl) +H]+; m/z = 208 [M(35Cl)-H]-; Rt = 2.30 min.

According to the analysis of related databases, 31230-17-8, the application of this compound in the production field has become more and more popular.

Synthetic Route of 31108-57-3, A common heterocyclic compound, 31108-57-3, name is 1H-Pyrazole-4-carbonitrile, molecular formula is C4H3N3, 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.

To a mixture of ABl (100 mg, 0.235 mmol) and K2C03 (64.9 mg, 0.47 mmol) in acetone (5 mL) was added lH-pyrazole-4-carbonitrile (32.7 mg, 0.352 mmol) at 25C. The reaction mixture was stirred at the 25C for 16 h. Then saturated aqueous H20 (50 mL) was added .The mixture was extracted with EtOAc (3 x 50 mL). The combined organic solution was washed with brine (20 mL), dried over Na2S04 and concentrated in vacuum to give the crude product .The crude product was purified by flash column (0-30% of EtOAc in PE) to give Compound 66 (38 mg, 37%) as a solid. (0895) 1H NMR (400 MHz, CDC13) delta 7.86 (s, 1H), 7.81 (s, 1H), 5.00 (d, J = 16.0 Hz, 1H), 4.85 (d, J = 16.0 Hz, 1H), 2.71-2.68 (m, 1H), 2.18-2.09 (m, 1H), 1.98-1.96 (m, 1H), 1.65-1.53 (m, 2H), 1.52-1.50 (m, 5H), 1.37-1.14 (m, 14H), 0.97 (d, J= 8 Hz, 4H), 0.85-0.81 (m, 1H), 0.75 (s, 3H), 0.68 (s, 3H). (0896) LCMS Rt = 2.594 min in 4.0 min chromatography, 30-90AB_220&254.1cm, purity 100%, MS ESI calcd. for C27H38N3O [M+H-H20]+ 420, found 420.

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.

Reference of 31108-57-3, 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. 31108-57-3, name is 1H-Pyrazole-4-carbonitrile, This compound has unique chemical properties. The synthetic route is as follows.

Compound D (140 mg, 0.27 mmol) was dissolved in DMF (5 ml), then sodium carbonate (50 mg, 0.54 mmol), 1H-pyrazole-4-carbonitrile (57 mg, 0.54 mmol) was added, and the reaction was carried out at 25 C for 4 hours. . Pour into 1N NaOH aqueous solution (20 ml), extract EA four times (30ml x 4), wash twice with 1N hydrochloric acid (30ml x 2), Dry over anhydrous sodium sulfate, After concentration, silica gel column chromatography gave 30 mg of a colorless oily viscous liquid 2-1. The yield was 26%.

The chemical industry reduces the impact on the environment during synthesis 1H-Pyrazole-4-carbonitrile. I believe this compound will play a more active role in future production and life.

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. 1192-21-8, name is 1-Methyl-1H-pyrazol-5-amine, This compound has unique chemical properties. The synthetic route is as follows., Product Details of 1192-21-8

2nd Generation XantPhos precatalyst (26.4 mg, 0.03 mmol) was added to (5)-2-(2,5- dichloropyrimidin-4-yl)-6-methyl-7-((6-methylpyridin-2-yl)methyl)-6,7- dihydroimidazo[l,2-a]pyrazin-8(5H)-one (Intermediate 46; 120 mg, 0.30 mmol), 1-methyl- lH-pyrazol-5-amine (72.2 mg, 0.74 mmol) and Cs2C03 (194 mg, 0.60 mmol) in 1,4- dioxane (8 mL) at 25 ¡ãC under nitrogen. The resulting mixture was stirred at 100 ¡ãC for 8 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. Pure fractions were evaporated to dryness to afford a yellow residue. This residue was further purified by preparative HPLC (XSelect CSH Prep CI 8 OBD column, 5mu silica, 19 mm diameter, 150 mm length), using decreasingly polar mixtures of water (containing 0.03percent NH3) and MeCN as eluents. Fractions containing the desired compound were evaporated to dryness to afford (5)-2-(5-chloro-2-((l-methyl-lH-pyrazol-5-yl)amino)pyrimidin-4-yl)-6- methyl-7-((6-methylpyridin-2-yl)methyl)-6,7-dihydroimidazo[l,2-a]pyrazin-8(5H)-one (Example 11; 50 mg, 36.2percent) as a white solid. H NMR (400 MHz, DMSO, 22 ¡ãC) delta 1.19 (3H, d), 2.47 (3H, s), 3.70 (3H, s), 4.08 (IH, d), 4.32 – 4.43 (2H, m), 4.53 (IH, dd), 5.15 (IH, d), 6.31 (IH, d), 7.21 (2H, dd), 7.34 (IH, d), 7.68 (IH, t), 8.21 (IH, s), 8.53 (IH, s), 9.72 (IH, s). m/z (ES+), [M+H]+ = 464

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 1192-21-8.

Adding a certain compound to certain chemical reactions, such as: 35344-95-7, name is 1H-Pyrazole-4-carbaldehyde, 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 35344-95-7, category: pyrazoles-derivatives

NaH (60% in oil, 79 mg, 2.0 mmol) was added to a solution of Intermediate 7(172 mg, 1.79 mmol) in DMF (18 mL) at 0C, and the reaction was allowed to stir at 0Cfor 15 minutes. A solution of 4-(bromomethyl)-1,1?-biphenyl (442 mg, 1.79 mmol) in 5mL of DMF was then added at 0C. The reaction stirred at 0 C for 1.5 hours, then allowed to warm to rt, and stirred for 5 minutes before quenching with water. The reaction was diluted with EtOAc, washed with 10% aq. LiC1 solution and brine, dried with Na2SO4, filtered and concentrated. The crude mixture was purified by silica gelchromatography to yield 39A (424 mg, 90.3%) as a white solid. MS(ESI) m/z 397.9 (M+H)h

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1H-Pyrazole-4-carbaldehyde, and friends who are interested can also refer to it.

Electric Literature of 930-36-9, 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 930-36-9 as follows.

The 6-[4-[4-[2-(l-methyl-lH-pyrazol-5-yl)ethoxy]phenyl]piperidin-l-yl]-3-(trifluoromethyl)[l,2,4]triazolo[4,3-b]pyridazine used as starting material was prepared as follows :-; Preparation of 2-(l-methyl-lH-pyrazol-5-yl)ethanol n-Butyl lithium (1.6M in hexanes) (1226 mL, 1961.78 mmol) was added dropwise to 1- methyl-lH-pyrazole (153.4 g, 1868.37 mmol) in THF (3000 mL) cooled to -78C over a period of 1 hour under nitrogen. The resulting solution was stirred at -600C for 30 minutes, then warmed to -100C and stirred for a further 40 minutes. A solution of oxirane (210 mL, 4203.82 mmol) in THF (600 mL) was added slowly at – 100C followed by further THF (1000 mL) and the resulting slurry was stirred at -100C for 30 minutes, then at 00C for 30 minutes. The mixture was then allowed to gradually warm to room temp under nitrogen and stirred for 16 hours. The reaction mixture was quenched with saturated NH4CI solution (2000 ml), the layers separated and the aqueous phase extracted with n-butanol (3 x 1000 ml). The combined organics were washed with saturated brine (1500 ml), dried over MgSOphi filtered and evaporated to give an oil, which was azeotroped with toluene(1000 ml) to leave an oil with some solid. The oil was dissolved in DCM and the insoluble solid was filtered off and washed with DCM. The filtrate was purified by chromatography using a silica Novasep prep HPLC column, eluting with a gradient of 5-10% methanol in DCM. Pure fractions were evaporated to dryness to afford 2-(l-methyl-lH-pyrazol-5- yl)ethanol (195 g, 83%) as an oil.IH NMR (400.1 MHz, DMSO-d6) delta 2.77 (2H, t), 3.63 (2H, m), 3.74 (3H, s), 4.74 (IH, t), 6.04 (IH, m), 7.26 (IH, d).

According to the analysis of related databases, 930-36-9, the application of this compound in the production field has become more and more popular.

Electric Literature of 31108-57-3, The chemical industry reduces the impact on the environment during synthesis 31108-57-3, name is 1H-Pyrazole-4-carbonitrile, I believe this compound will play a more active role in future production and life.

To a solution of IV-B8 (44 mg, 0.11 mmol) in acetone (2 mL) was added lH-pyrazole-4- carbonitrile (16 mg, 0.17 mmol) and K2C03 (48 mg, 0.34 mmol). After stirring at 25C for 12 h, the mixture was diluted with water (5 mL) and extracted with EtOAc (2 x 10 mL). The combined organic solution was washed with brine (5 mL), dried over anhydrous Na2S04, filtered and concentrated. The residue was purified by flash column (0-43% of EtOAc in PE) to give IV-B9 (22 mg, 49%) as a solid. (3084) 1HNMR (400 MHz, CDCl3) dH 7.86 (s, 1H), 7.81 (s, 1H), 5.08-5.02 (m, 1H), 4.94-4.87 (m, 1H), 2.63 (t, j= 8.8 Hz, 1H), 2.26-2.16 (m, 1H), 2.06-1.99 (m, 1H), 1.82-1.70 (m, 6H), 1.46- 1.17 (m, 15H), 0.91-0.83 (m, 2H), 0.65 (s, 3H). LC-ELSD/MS purity 99%, MS ESI calcd. for C24H33N302 [M+H]+396.2, found 396.2

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-4-carbonitrile, other downstream synthetic routes, hurry up and to see.

Reference of 14521-81-4, 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. 14521-81-4, name is 3-Fluoro-1H-pyrazole, This compound has unique chemical properties. The synthetic route is as follows.

To a stirred solution of 4, 6-dichloro-N-(4, 4-difluorocyclohexyl) pyrimidin-2-amine (1 g, 3.54 mmol) in acetonitrile (10 mL) was added 3-fluoro pyrazole (0.36 g, 4.25 mmol) and cesium carbonate (2.30 g, 7.089 mmol). The reaction mixture was heated at 80 C for 8h. The reaction mixture was filtered and the filtrate was concentrated to afford crude product and which was purified by column chromatography (60-120 mesh) using 22% ethyl acetate in pet ether as solvent to afford 4, 6-dichloro-N-(4, 4- difluorocyclohexyl) pyrimidin-2-amine [Bj as an off-white solid (4 g, 32%). MS (M, M+2)=282.0, 284.1.

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