Day: May 11, 2021

Application of 29004-73-7, 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. 29004-73-7, name is (3-methyl-1H-pyrazol-5-yl)methanol belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

To (+/-)-6′-methanesulfonyloxy-6-(3-methanesulfonyloxypropoxy)-4,4,4′,4′,7,7′-hexa-methyl-2,2′-spirobichroman (Ex. 4a, 2 g, 3.4 mmol) and (5-methyl-1H-pyrazol-3-yl)-methanol (0.77 g, 6.8 mmol) in 50 mL of DMF at room temperature was added sodium hydride (0.41 g, 10.3 mmol, 60% dispersion in mineral oil) portion-wise. This reaction mixture was stirred at room temperature for 2 h and poured into water. The precipitate was isolated by filtration and re-dissolved in 60 mL of MeOH/THF (1:1 v/v). To this solution was added 5 mL of 5 N NaOH and the resulting mixture was stirred at 70 C. overnight. The reaction mixture was acidified with 3 N HCl to pH=6 and concentrated to 25 mL. This mixture was extracted with dichloromethane and the combined organic extracts were washed with brine and water. Purification by silica gel chromatography (EtOAc/Hexane, 1:2) afforded two products. The slower eluting component gave 0.22 g of the title compound as a white solid, mp 217-219 C. 1H NMR (CDCl3): delta 6.73 (s, 1H), 6.67 (s, 1H), 6.47 (s, 1H), 6.45 (s, 1H), 5.99 (s, 1H), 4.64 (d, 2H, J=5.2 Hz), 4.46 (s, 1H), 4.22 (t, 2H, J=7.3 Hz), 3.93-3.88 (m, 2H), 2.32-2.27 (m, 2H), 2.23 (s, 3H), 2.10 (s, 6H), 2.06-1.89 (m, 4H), 1.56 (s, 6H), 1.31 (s, 6H). HRMS (EI) Calcd for C31H40N2O5: 520.2937 (M+); found: 520.2932.; Example 18 (+/-)-6′-Hydroxy-6-[3-(5-hydroxymethyl-3-methyl-1H-pyrazol-1-yl)propoxy]-4,4,4′,4′,7,7′-hexamethyl-2,2′-spirobichromanTo (+/-)-6′-methanesulfonyloxy-6-(3-methanesulfonyloxypropoxy)-4,4,4′,4′,7,7′-hexa-methyl-2,2′-spirobichroman (Ex. 4a, 2 g, 3.4 mmol) and (5-methyl-1H-pyrazol-3-yl)-methanol (0.77 g, 6.8 mmol) in 50 mL of DMF at room temperature was added sodium hydride (0.41 g, 10.3 mmol, 60% dispersion in mineral oil) portion-wise. This reaction mixture was stirred at room temperature for 2 h and poured into water. The precipitate was isolated by filtration and re-dissolved in 60 mL of MeOH/THF (1:1 v/v). To this solution was added 5 mL of 5 N NaOH and the resulting mixture was stirred at 70 C. overnight. The reaction mixture was acidified with 3 N HCl to pH=6 and concentrated to 25 mL. This mixture was extracted with dichloromethane and the combined organic extracts were washed with brine and water. Purification by silica gel chromatography (EtOAc/Hexane, 1:2) afforded two products. The faster eluting component gave 0.095 g of the title compound as a white solid, mp 208-210 C. 1H NMR (CDCl3): delta 6.73 (s, 1H), 6.67 (s, 1H), 6.46 (s, 1H), 6.44 (s, 1H), 5.99 (s, 1H), 4.72-4.80 (br, 1H), 4.60 (s, 2H), 4.31 (t, 2H, J=7.2 Hz), 3.92 (t, 2H, J=5.1 Hz), 2.36-2.29 (m, 2H), 2.26 (s, 3H), 2.10 (s, 3H), 2.09 (s, 3H), 2.06-1.87 (m, 4H), 1.56 (s, 6H), 1.30 (s, 6H). HRMS (EI) Calcd for C31H40N2O5: 520.2937 (M+); found: 520.2940.

The synthetic route of (3-methyl-1H-pyrazol-5-yl)methanol has been constantly updated, and we look forward to future research findings.

Synthetic Route of 128694-63-3, 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 128694-63-3 as follows.

Example 310 Production of N-[5-({2-[(cyclopropylcarbonyl)amino]imidazo[1,2-b]pyridazin-6-yl}oxy)-2-fluorophenyl]-1-methyl-3-(trifluoromethyl)-1H-pyrazole-5-carboxamide In the same manner as in Example 259 and using 1-methyl-3-(trifluoromethyl)-1H-pyrazole-5-carboxylic acid (150 mg, 0.79 mmol), tetrahydrofuran (5 mL), N,N-dimethylformamide (1 drop), oxalyl chloride (140 muL, 1.6 mmol), N-[6-(3-amino-4-fluorophenoxy)imidazo[1,2-b]pyridazin-2-yl]cyclopropanecarboxamide (200 mg, 0.61 mmol) and N,N-dimethylacetamide (7 mL) as starting materials, the title compound (240 mg, 77%) was obtained as a white solid. 1H-NMR (DMSO-d6, 300 MHz) delta 0.71-0.85 (4H, m), 1.85-1.97 (1H, m), 4.15 (3H, s), 7.09 (1H, d, J=9.4 Hz), 7.21-7.28 (1H, m), 7.39-7.47 (1H, m), 7.54 (1H, s), 7.58 (1H, dd, J=6.3, 2.9 Hz), 7.95 (1H, s), 8.05 (1H, d, J=9.4 Hz), 10.45 (1H, s), 11.08 (1H, s).

According to the analysis of related databases, 128694-63-3, the application of this compound in the production field has become more and more popular.

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. 873191-23-2, name is 5-(Bromomethyl)-1,3-dimethyl-1H-pyrazole, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C6H9BrN2

General procedure: The phenanthridine skeletons1-8 (0.1 mmol) were dissolved in dryTHF (10 mL), and NaH (50 mg, 2 mmol), and 3-(bromomethyl)pyridine,3-(chloromethyl)-1,5-dimethyl-1H-pyrazole or 5-bromomethyl-1,3-dimethyl-1H-pyrazole (1 mmol) were added. The mixture was stirred atrt. for 12 h and quenched with H2O (50 mL) in an ice bath. The solutionwas evaporated to remove the THF and extracted with CH2Cl2(2×30 mL). The organic layer was washed with saturated NaHCO3 andbrine, dried over MgSO4, filtered and concentrated. The residue waspurified by column chromatography using petroleum-EtOAc as theeluent to afford about 35 mg of each phenanthridine compound.

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 873191-23-2.

Related Products of 73387-52-7, These common heterocyclic compound, 73387-52-7, name is 5-(4-Bromophenyl)-1-methyl-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.

Step 4: Preparation of 4-(3-{[4-(1-methyl-1H-pyrazol-5-yl)phenyl]thio]phenyl) tetrahydro-2H-pyran-4-carboxamide A mixture of 5-(4-bromophenyl)-1-methyl-1H-pyrazole (0.50 g, 2.10 mmols,), 4-{3-[(tri-isopropylsilyl)thio]phenyl}tetrahydro-2H-pyran-4-carboxamide (0.83 g, 2.10 mmols), Tetrakis(triphenylphosphine)palladium(0) (243 mg, 0.10 equivalents), bis[(2-diphenyl-phosphino)]phenyl ether (113 mg, 0.10 equivalents), and 1.0 M potassium tert-butoxide in THF (6.3 mmols, 3 equivalents) in iPrOH (15 mL) that contained 5% water was heated for 4 hours at 90 degrees Celcius in an atmosphere of nitrogen. The reaction mixture was cooled to room temperature and 7 mL of 1N HCl was added. The product was precipitated by the addition of water (30 mL). The precipitate was collected by suction filtration and washed with water (2*20 mL) and cold ethyl ether (4*20 mL). The tan brown solid was dissolved in a small volume of methylene chloride containing 1% methanol and applied to a 140 g cartridge of silica gel. The cartridge was eluted with an acetone:hexane gradient. The appropriate fractions were concentrated and triturated with methanol to produce a white solid (710 mg) as product. 1H NMR (400 MHz, DMSO-d6) delta ppm 1.75-1.84 (m, 3H) 2.40 (d, J=13.54 Hz, 3H) 3.43-3.51 (m, 1H) 3.72 (d, J=11.34 Hz, 3H) 3.84 (s, 3H) 6.40 (d, J=1.46 Hz, 1H) 7.02 (s, 1H) 7.22-7.30 (m, 2H) 7.34 (d, J=8.05 Hz, 1H) 7.38-7.43 (m, 2H) 7.45-7.52 (m, 3H). HRMS calc M+H, 394.1589, found 394.1630.

Statistics shows that 5-(4-Bromophenyl)-1-methyl-1H-pyrazole is playing an increasingly important role. we look forward to future research findings about 73387-52-7.

Adding a certain compound to certain chemical reactions, such as: 139756-04-0, name is 1-Methyl-4-(2-propoxybenzamido)-3-propyl-1H-pyrazole-5-carboxamide, 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 139756-04-0, COA of Formula: C18H24N4O3

In step 1, 4-[2-propyloxy-5-(chlorosulfonyl)benzamido] – l-methyl-3-propyl-5-carbamoyl pyrazole is prepared. Precisely, the proper amount of 4-[2-propyloxy benzamido]-l-methyl-3-propyl-5-carbamoyl pyrazole is added to the solution of the proper amount of chlorosulfonic acid cooled at 0 0C. The mixture is stirred, filtered, washed and dried to give 4-[2-propyloxy-5-(chlorosulfonyl)benzamido ]- l-methyl-3-propyl-5-carbamoyl pyrazole.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Methyl-4-(2-propoxybenzamido)-3-propyl-1H-pyrazole-5-carboxamide, and friends who are interested can also refer to it.

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. 19959-77-4, name is 2-(5-Methyl-1H-pyrazol-3-yl)pyridine, A new synthetic method of this compound is introduced below., category: pyrazoles-derivatives

Solid ligand L (0.2mmol, 31.8mg) and Cd(NO3)2·4H2O (0.1mmol, 30.8mg) were placed into the bottom of separate arms of an H-tube. The H-tube was filled with acetonitrile solution and sealed with plastic film. After one week, colorless stick-like crystals of compound 4 were generated and collected, washed with n-hexane 2-3 times, then dried in vacuum. Yield: 42.72mg (77%), M. p. > 300C. Anal. Calc. for C18H18CdN8O6 (FW, 554.8): C, 38.97; H, 3.27; N, 20.20. Found: C, 38.31; H, 3.39; N, 19.70%. Selected IR data (cm-1, KBr): 3200 (b, s), 3135 (s), 2994 (s), 2853 (m), 2363 (s), 1607 (m) (nu(C=N)), 1578 (m) (nu(C=C)), 1435 (s), 1387 (s), 1340 (m), 1301 (m), 1225 (w), 1156 (w), 1111 (w), 1018 (w), 980 (s), 797 (s), 740 (m).

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.

Adding a certain compound to certain chemical reactions, such as: 304693-70-7, name is 1-(2-Methoxyethyl)-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 304693-70-7, Product Details of 304693-70-7

In a sealed tube, under N2, intermediate 35 (211 mg; 1.37 mmol) and Ti(OiPr)4 (436 jiL; 1.83 mmol) were added to a solution of intermediate 11(300mg; 0.914 mmol) in THF(6 mL). The solution was stirred at 50C for 5 hours then at rt overnight. The reaction mixture was cooled to 5C and isopropyl magnesium chloride 2M in THF (2.28 mL; 4.57 mmol) was added dropwise. The reaction mixture was allowed to rise slowly to rt and stirred overnight. The reaction mixture was diluted with EtOAc and poured onto a 10% aqueous solution of K2C03. The precipitate was removed by filtration over Celite. Theorganic layer was decanted, washed with brine, dried over MgSO4, filtered and evaporated to dryness. The residue was purified by chromatography over silica gel (irregular SiOH, 40g; mobile phase: gradient from 0% MeOH, 100% DCM to 10% MeOH, 90% DCM). The fractions containing the product were collected and evaporated to dryness to give 0.337 g of an intermediate residue which was purified again bychromatography via reverse phase (stationary phase: YMC-actus Triart C18 lOjim30*150mm, mobile phase: gradient from 55% NH4HCO3 0.2%, 45% ACN to 0%NH4HCO3 0.2%, 100% ACN). The pure fractions were collected and evaporated todryness. The residue was freeze-dried with acetonitrile/water 20/80 to afford 120 mg(26%) of compound 71.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-(2-Methoxyethyl)-1H-pyrazole-4-carbaldehyde, and friends who are interested can also refer to it.

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. 1125828-30-9, name is 1-(4-Chloro-2-(3-methyl-1H-pyrazol-1-yl)phenyl)-2,2,2-trifluoroethanone, A new synthetic method of this compound is introduced below., Computed Properties of C12H8ClF3N2O

6.2. Preparation of (R)-1-(4-chloro-2-(3-methyl-1H-pyrazol-1-yl)phenyl)-2,2,2-trifluoroethanol A 3 L 3-neck jacketed round bottom flask equipped with a mechanical stirrer, a temperature controller, and a nitrogen inlet was charged sequentially with dichloro(pentamethylcyclopentadienyl)iridium (III) dimer ([Cp*IrCl2]2, STREM, CAS#: 12354-85-7, 34 mg, 0.043 mmol), (1R,2R)-(-)-N-(4-toluenesulfonyl)-1,2-diphenylethylenediamine (STREM, CAS#: 144222-34-4, 32 mg, 0.087 mmol), and water (400 mL, 4*) at room temperature. The resulting mixture was stirred for 3 hours at 40 C. to give a homogeneous orange solution. To this active catalyst solution was added potassium formate (145.5 g, 1.73 mol) and a solution of the ketone 1-(4-chloro-2-(3-methyl-1H-pyrazol-1-yl)phenyl)-2,2,2-trifluoroethanone (100 g, >99% purity by GC, 0.346 mol) in CH3CN (500 mL, 5*) at 40 C. The reaction mixture was then stirred at 40 C. for 2 h at which time the reaction was determined to be complete by GC. After cooled to 30 C., the aqueous layer (ca. 480 mL) was removed. The organic layer (ca. 600 mL, 6*) was treated with activated carbon (Darco G-60, 20 g, 0.2*) at 45 C. for 2 h and filtered through 1/4 inch bed of Celpure P65 (USP-NF, Pharmaceutical grade, Sigma) and washed with CH3CN (200 mL, 2*). The filtrate was concentrated to 250 mL (2.5*) and transferred to a 2 L 3-neck jacketed round bottom flask equipped with a mechanical stirrer and a temperature controller. More CH3CN (50 mL, 0.5*) was added to increase the solution volume to 300 mL (3*). This solution was warmed to 60 C. and water (500 mL, 5*) was added to this solution at the same temperature. After stirred for 15 minutes at 60 C., the resulting emulsion-like milky mixture was slowly cooled to room temperature. The crystals were then filtered at room temperature, and washed with CH3CN/water (1:2, 150 mL, 1.5*). The wet cake (108 g, KF: 8.83%) was dried under vacuum at 45 C. for 4 h to afford the desired alcohol (white solid, 95 g, 94% yield, >99% chemical purity, >99% ee, KF: 0.014%).

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.

Synthetic Route of 128694-63-3, A common heterocyclic compound, 128694-63-3, name is 1-Methyl-3-(trifluoromethyl)-1H-pyrazole-5-carboxylic acid, molecular formula is C6H5F3N2O2, 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.

EXAMPLE 2 N-[5-(2-chloro-6-fluorophenyl)-1H-pyrazol-3-yl]-1-methyl-3-(trifluoromethyl)-1H-pyrazole-5-carboxamide [0113] Compound of Preparation 11 (100 mg, 0.19 mmol) and 1-methyl-3-(trifluoromethyl)-1 H-pyrazole-5-carboxylic acid (91 mg, 0.47 mmol) were dissolved in 1.5 mL DMF. N-(3-Dimethylaminopropyl)-N’-ethylcarbodiimide hydrochloride 98% (144 mg, 0.75 mmol) and 1-Hydroxybenzotriazole hydrate (102 mg, 0.75 mmol) were added and the mixture was stirred at room temperature overnight. Ethyl acetate was added and the organic phase was washed with water two times, NaOH 1 N two times, dried over MgSO4 and evaporated under reduced pressure and the residue was purified using the Isolera purification (ethyl acetate – hexane gradient, 0:100 rising to 100:0) to give 35 mg (0.09 mmol, 19%) of the title compound as a white solid. LRMS (m/z): 388 (M+1)+. 1 H NMR (300 MHz, DMSO-d6) d ppm 4.19 (3 H, s), 6.86 (1 H, s), 7.31 – 7.61 (3 H, m), 7.65 (1 H, s), 11.24 (1 H, br. s), 12.97 (1 H, br. s)

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.

Some common heterocyclic compound, 128694-63-3, name is 1-Methyl-3-(trifluoromethyl)-1H-pyrazole-5-carboxylic acid, molecular formula is C6H5F3N2O2, 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. SDS of cas: 128694-63-3

BB4; 5-(chloromethyl)-l-methyl-3-(trifluoromethyl)-lH-pyrazoleBB4a BB4b BB4Step A: l-Methyl-3-(trifluoromethyl)-lH-pyrazole-5-carboxylic acid BB4a (837 mg, 4.3 mmol) is dissolved in anhydrous tetrahydrofurane (10 mL), then LiAlH4 (2.16 mL of 2.0 M in tetrahydrofurane, 4.3 mmol) is added dropwise and stirred at rt for lh. The mixture is quenched by dropwise addition of IN HC1, then is made basic by addition of saturated NaHC03 and extracted with EtOAc (3x). The organic layers are combined, washed with brine, dried (MgS04), filtered and concentrated to provide (l-methyl-3-(trifluoromethyl)- lH-pyrazol-5-yl)methanol BB4b as a clear oil. 1H NMR (400 MHz, CDC13) delta = 6.46 (s, 1H), 4.69 (d, J = 5.6 Hz, 2H), 3.95 (s, 3H); MS calcd. for C6H8F3N20 ([M+H]+): 181.0, found: 181.1.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 128694-63-3, its application will become more common.