Tag: M.W=0-100

3920-50-1, 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. 3920-50-1 name is Pyrazole-3-carboxaldehyde, 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.

3.9 mg of 1H-pyrazole-3-carboxaldehyde was added to a dimethylformamide (0.5 ml) solution of 15 mg of 4-(2-fluoro-phenoxy)-5-(6-methanesulfonyl-pyridin-3-yloxy)-benzene-1,2-diamine obtained in Example 200, and the reaction liquid was stirred at 90¡ãC for 30 minutes. The solvent was evaporated away under reduced pressure, and the resulting residue was purified through partitioning thin-layer chromatography (Kieselgel.(TM). 60F254, Art 5744 (by Merck), chloroform/methanol = 9/1) to obtain the entitled compound as a white solid. 1HNMR(CDCl3)delta: 3.20(3H,s), 6.94-6.99(1H,m), 7.01-7.15(4H,m), 7.25-7.65(2H,m), 7.31(1H,dd,J=8.9,2.7Hz), 7.66(1H,d,J=2.3Hz), 7.98(1H,d,J=8.9Hz), 8.40(1H,d,J=2.7Hz) ESI-MS(m/e):466[M+H]

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Pyrazole-3-carboxaldehyde, and friends who are interested can also refer to it.

1192-21-8, name is 1-Methyl-1H-pyrazol-5-amine, 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. 1192-21-8

(R)-2-(2-Chloro-5-methylpyrimidin-4-yl)-6-m yl)methyl)-6,7-dihydroimidazo[l ,2-a]pyrazin-8(5H)-one (Intermediate 91 ; 187 mg, 0.43 mmol), 1 -methyl- lH-pyrazol-5-amine (104 mg, 1.07 mmol),Cs2C03 (279 mg, 0.86 mmol) and 2nd Generation XantPhos precatalyst (38.0 mg, 0.04 mmol) in 1 ,4-dioxane (5 mL) was stirred under an atmosphere of nitrogen at 1 10 ¡ãC for 16 hours. The solvent was removed by distillation under vacuum. The crude product was purified by flash silica chromatography, elution gradient 3 to 5percent MeOH in DCM. The product was further purified by preparative HPLC (XSelect CSH Prep C 18 OBD column, 5mu silica, 19 mm diameter, 150 mm length), using decreasingly polar mixtures of water (containing 0.01percent NH4HCO3) and MeCN as eluents. Fractions containing the desired compound were evaporated to dryness to afford (i?)-6-methyl-2-(5-methyl-2-((l-methyl-lH-pyrazol-5- yl)amino)pyrimidin-4-yl)-7-((6-(trifluoromethyl)pyridin-2-yl)methyl)-6,7- dihydroimidazo[l ,2-a]pyrazin-8(5H)-one (1 12 mg, 52.6percent) as a white solid. lH NMR (400 MHz, DMSO, 20.9 ¡ãC) delta 1.22 (3H, d), 2.52 (3H, s), 3.35 (1H, s), 3.71 (3H, s), 4.13 (1H, ddd), 4.40 (IH, dd), 4.51 – 4.63 (2H, m), 5.22 (IH, d), 6.31 (IH, d), 7.34 (IH, d), 7.78 (IH, d), 7.84 (IH, d), 7.97 (IH, s), 8.10 (IH, t), 8.33 (IH, d), 9.24 (IH, s). m/z (ES+), [M+H]+ = 498.

Statistics shows that 1192-21-8 is playing an increasingly important role. we look forward to future research findings about 1-Methyl-1H-pyrazol-5-amine.

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.

1120-82-7, Adding some certain compound to certain chemical reactions, such as: 1120-82-7, name is (1H-Pyrazol-1-yl)methanol, 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 1120-82-7.

Analogous method is applied for synthesis of LB as described for LA. The CH2Cl2 solution (10.0mL) of 2,6-diethylbenzenamine (3.29mL, 0.0200mol) was added a CH2Cl2 solution (30.0mL) of 1H-1-pyrazolyl-1-methanol (3.92g, 0.0400mol). The reaction solution was dried over the MgSO4 after stirring the reaction mixture at room temperature for 3days. The filtrate solvent was removed under reduced pressure to give bright yellow oil (5.54g, 89.5%). Anal. Calc. for C18H23N5: C, 69.8; H, 7.49; N, 22.6. Found: C, 68.1; H, 7.41; N, 21.6%. 1H NMR (CDCl3, 400MHz): delta 7.57 (d, 2H, J=2.0Hz, -N=CH-CH=CH-N-), 7.28 (d, 2H, J=2.0Hz, -N=CH-CH=CH-N-), 7.19 (t, 1H, J=7.2Hz, p-NC6H3(CH2CH3)2-), 7.09 (d, 2H, J=7.6Hz, m-NC6H3(CH2CH3)2-), 6.24 (t, 2H, J=2.0Hz, -N=CH-CH=CH-N-), 5.40 (s, 4H, -N-CH2-N-), 2.10 (q, 4H, J=7.6Hz, -NC6H3(CH2CH3)2-), 1.05 (t, 6H, J=7.6Hz, -NC6H3(CH2CH3)2-). 13C NMR (CDCl3, 100MHz): delta 142.94 (s, 1C, ipso-NC6H3(CH2CH3)2), 142.41 (s, 2C, o-NC6H3(CH2CH3)2-), 139.90 (d, 2C, J=183Hz, -N=CH-CH=CH-N-), 129.27 (d, 2C, J=184Hz, -N=CH-CH=CH-N-), 127.25 (d, 2C, J=158Hz, m-NC6H3(CH2CH3)2-), 126.42 (d, 1C, J=156Hz, p-NC6H3(CH2CH3)2-), 105.95 (d, 2C, J=176Hz, -N=CH-CH=CH-N-), 68.85 (t, 2C, J=149Hz, -N-CH2-N-), 23.00 (t, 2C, J=125Hz, -NC6H3(CH2CH3)2-), 14.75 (q, 2C, J=125Hz, -NC6H3(CH2CH3)2-). IR (liquid neat; cm-1): 3845 (w), 3743 (w), 3617 (w), 3110 (w), 2967 (m), 1702 (w), 1151 (m), 1457 (m), 1392 (m), 1264 (s), 1159 (s), 1083 (s), 1042 (s), 962 (m), 873 (w), 812 (w), 744 (s), 653 (w), 616 (m), 581 (w).

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 1120-82-7.

35344-95-7, A common heterocyclic compound, 35344-95-7, name is 1H-Pyrazole-4-carbaldehyde, molecular formula is C4H4N2O, 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 stirred solution of 1H- pyrazole-4-carbaldehyde 13-4 (220 mg, 2.29 mmol) in DMF (5 mL) was added cesium carbonate (1.86 g, 5 72 mmol) and cyclohexyl methanesulfonate 13-3 (489.74 mg, 2.75 mmol). The reaction mixture was heated at 60C for 16 hours. The reaction mixture was quenched with cold water and extracted with ethyl acetate. The organic layer was washed with a saturated aqueous solution of NaHCCb, dried over NaiSCh and concentrated under reduced pressure to afford crude which was purified by column chromatography to afford l-cyclohexylpyrazole-4-carbaldehyde 13-5 (220 mg, 1.23 mmol, 53.91 % yield) as gummy liquid. LC MS: ES+ 179.

The synthetic route of 35344-95-7 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. 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.

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.

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 1072-68-0 as follows. 1072-68-0

To a solution of 1,4-dimethyl-1H-pyrazole (52 g, 541 mmol) in anhydrous THF (1.0 L) was added dropwise n-BuLi (0.22 L, 2.5 M, 550 mmol) at -78 C with stirring over 2 h. Then, a solution of (RS)-4 (110 g, 396 mmol) in anhydrous THF (1.0 L) was added dropwise to the above solution over 1 h at the same temperature. The resulting mixture was stirred at -78 C for 1.5 h. TLC (PE-EtOAc, 1:2) showed (RS)-4 was completely consumed. The mixture was poured into sat. aq NH4Cl (1 L) and extracted with EtOAc (3 ¡Á 0.8 L). The combined organic extracts were washed with brine (1 L), dried (Na2SO4), and concentrated to give the crude product. Purification by column chromatography on silica gel (PE-EtOAc, 20:1 ? 5:1) gave 8i as a yellow oil, and 7i as a yellow solid when the column was continuously eluted with PE-EtOAc(5:1 ? 2:1).

According to the analysis of related databases, 1072-68-0, 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. 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. 35277-02-2

3-(3-(4-(chloromethyl)benzyl)isoxazol-5-yl)pyridin-2 -amine (Intermediate B, 80mg, 0.27mmol) and 4-fluoro-lH-pyrazole (92mg, l .07mmol) were dissolved in NMP (lml). Potassium 2-methylpropane- 2-olate (1M in THF, 0.80mL, 0.80mmol) was added and the mixture was stirred for 5min at 60C. The cooled reaction mixture was directly purified by column chromatography (Si02, hexane/ethyl acetate). Fraction containing the product were concentrated under reduced pressure and further purified by HPLC to yield 3-(3-(4-((4-fluoro-lH-pyrazol-l-yl)methyl)benzyl)isoxazol-5-yl)pyridin-2-amine (75mg, 0.22mmol, 80%) as a white solid. 400 MHz NMR (CDCl3) d 8.14 (s, 1H), 7.69 (dd, J= 7.7, 1.7 Hz, 1H), 7.35 (dd, J= 4.3, 0.8 Hz, 1H), 7.31 – 7.13 (m, 5H), 6.70 (dd, J= 7.7, 4.7 Hz, 1H), 6.24 (s, 1H), 5.43 (s, 2H), 5.18 (s, 2H), 4.04 (s, 2H). MS: 350.3 [M+H]+.

The synthetic route of 35277-02-2 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. 1072-68-0, name is 1,4-Dimethylpyrazole, A new synthetic method of this compound is introduced below., 1072-68-0

To a solution of 1,4-dimethyl-1H-pyrazole (2.5 g, 26.0 mmol, 1 equiv) in tetrahydrofuran (50 mL) was added n-butyllithium in hexane solution (2.5 M in hexane, 78.0 mmol, 31 mL, 3 equiv) dropwise at 0 C. under nitrogen atmosphere. The resulting solution was stirred at room temperature for 1 h and then cooled to -78 C. 2-isopropoxy-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (14.52 g, 78.017 mmol, 3 equiv) was added and the reaction mixture was stirred at -78 C. for 0.5 hour, then slowly warmed up to 0 C. The reaction was quenched with brine and extracted with EtOAc (250 mL*3). The combined organic layer was washed with brine, dried over Na2SO4 and concentrated under reduced pressure. The residue was applied onto a silica gel column eluting with ethyl acetate/petroleum ether (1:5). This resulted in 2.6 g (45%) of 1,4-dimethyl-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazole as a white solid.

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.