Day: March 3, 2021

Adding a certain compound to certain chemical reactions, such as: 326827-21-8, name is 3-Amino-5-cyclobutyl-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 326827-21-8, category: pyrazoles-derivatives

Example 297: Preparation of N2-(lH-benzo[d]imidazol-6-yl)-N4-(5-cyclobutyl-lH-pyrazol- 3-yl)-5-(trifluoromethyl)pyrimidine-2,4-diamine2,4-Dichloro-5-(trifluoromethyl)pyrimidine (0.087 g, 0.401 mmol), 5-cyclobutyl-lH- pyrazol-3-amine (0.055 g, 0.401 mmol) and N-ethyl-N-isopropylpropan-2-amine (0.077 ml,0.441 mmol) were mixed in acetonitrile (2 ml). The mixture was microwaved at 80 C for 20 min and then concentrated. lH-benzo[d]imidazol-6-amine (0.053 g, 0.401 mmol) and acetic acid (0.024 g, 0.401 mmol) were added. The mixture was microwaved at 110 C for 20 min and then concentrated. 14 mg of product was recovered after automated reverse phase chromatography (water-MeCN). MS calcd for [Ci9Hi7F3N8+H]+: 415.16, found 415.20.

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, 3-Amino-5-cyclobutyl-1H-pyrazole, other downstream synthetic routes, hurry up and to see.

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. 133228-21-4, name is N,N-Dimethyl-1H-pyrazole-1-sulfonamide, A new synthetic method of this compound is introduced below., category: pyrazoles-derivatives

Step A: Preparation of 3~bromo-N,N-dimethyl-lH-pyrazole-l-sulfonamide; To a solution of N,N-dimethylsulfamoylpyrazole (44.O g, 0.251 mol) in dry tetrahydrofuran (500 mL) at -78 0C was added dropwise a solution of n-butyllithium (2.5 M in hexane, 105.5 mL, 0.264 mol) while maintaining the temperature below -60 C. A thick solid formed during the addition. Upon completion of the addition the reaction mixture was stirred at -78 C for an additional 15 minutes, after which time a solution of 1,2-dibromo- tetrachloroethane (90 g, 0.276 mol) in tetrahydrofuran (150 mL) was added dropwise while maintaining the temperature below -70 0C. The reaction mixture turned a clear orange; stirring was continued for an additional 15 minutes. The -78 0C bath was removed and the reaction was quenched with water (600 mL). The reaction mixture was extracted with methylene chloride (4x), and the organic extracts were dried over magnesium sulfate and concentrated. The crude product was further purified by chromatography on silica gel using methylene chloride-hexane (50:50) as eluent to afford 57.04 g of the title product as clear colorless oil. 1H NuMR (CDCl3): delta 7.62 (m,lH), 6.44 (m,lH), 3.07 (d,6H).

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: 1222174-92-6, name is Methyl 5-bromo-1-methyl-1H-pyrazole-3-carboxylate, 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 1222174-92-6, Recommanded Product: Methyl 5-bromo-1-methyl-1H-pyrazole-3-carboxylate

A solution of intermediate 2a (515 mg), 2,5-dimethoxyphenylboronic acid (642 mg) and Pd(dppf)Cl2.CH2Cl2 (105 mg) in a mixture of THF (15 mL) and sodium carbonate solution (2 M, 3 mL) was heated in a microwave (Biotage) to 100 C. for 1.5 h. The mixture was chilled, the layers separated and the aqueous layer was extracted with EtOAc. The combined organic layers were dried and the volatiles were removed under reduced pressure. The residue was purified by chromatography (Interchim cartridge 50SiHP/25 g, Cy/EtOAc) to yield the desired compound (77% yield). [0349] LC-MS (Method 2): m/z [M+H]+=277.1 (MW calc.=276.29); Rt=0.62 min.

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, Methyl 5-bromo-1-methyl-1H-pyrazole-3-carboxylate, other downstream synthetic routes, hurry up and to see.

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. 81945-73-5, name is 1H-Pyrazol-1-ol, A new synthetic method of this compound is introduced below., Recommanded Product: 81945-73-5

(General Procedure 16)4-Benzo[1,3]dioxol-5-yl-piperazine-1-carboxylic Acid pyrazol-1-yl Ester The title compound was prepared from 1-hydroxypyrazole and 1-Benzo[1,3]dioxol-5-ylpiperazine applying the general procedure 16. The crude product was purified by flash chromatography (Quad flash 12, EtOAc-heptane) (92%, crystals). 1H NMR (300 MHz; CDCl3): delta 3.11 (bt, 4H), 3.71 (bs, 2H), 3.83 (bs, 2H), 5.93 (s, 2H), 6.32 (t, 1H), 6.39 (dd, 1H), 6.57 (d, 1H), 6.74 (d, 1H), 7.37 (dd, 1H), 7.41 (dd, 1H); HPLC-MS: m/z=317.2 (M+1); Rt=2.96 min.

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.

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. 930-36-9, name is 1-Methylpyrazole belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below. Formula: C4H6N2

Step 1; [00116] q-Methyl-lH-pyrazol-5-yl)phihenyl)methanol: At about -78 0C, n- butyllithium (58.5 mL, 2.5M) was added to a solution of 1 -methyl- lH-pyrazole (10 g, 121.95 mmol, 1.00 equiv.) in tetrahydrofuran (200 mL). The mixture was stirred at about -78 0C for about 1 hour, and then benzaldehyde (14.2 g, 133.96 mmol, 1.10 equiv.) was added. The mixture was stirred at ambient temperature for about 16 hours, and then a saturated aqueous solution of ammonium chloride (100 mL) was added. Following standard extractive workup with ethyl acetate (2 x 100 mL), the resulting residue was purified by silica gel column chromotagraphy (ethyl acetate / petroleum ether (1:1)) to give the title product as a white solid (20.2 g; yield = 88%). LC-MS: m/z = 189 (MH)+. 1H NMR (300 MHz, CHCl3) delta: 7.26-7.38 (m, 6H), 6.00 (d, / = 1.8 Hz, IH), 5.85 (s, IH), 3.70 (s, 4H).

The synthetic route of 930-36-9 has been constantly updated, and we look forward to future research findings.

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. 5334-39-4, name is 3-Methyl-4-nitro-1H-pyrazole, This compound has unique chemical properties. The synthetic route is as follows., category: pyrazoles-derivatives

To a solution of 3-methyl-4-nitro-lH-pyrazole (3.81 g, 30.0 mmol) in DMF (20 mL) was added K2CO3 (8.28 g, 60.0 mmol) and diethyl 2-bromo-2-methylmalonate (9.10 g, 36.0 mmol). The mixture was stirred at 100 C for 20 h. The reaction mixture was then treated with H20 (500 mL), extracted with ethyl acetate (20 mL x 3). The organic layer was evaporated and the residue was purified by silica gel column chromatography eluting with petroleum ether/ethyl acetate (10/1) to afford the title compound (3.6 g, 41%) as oil. LC-MS (ESI): m z = 300 (M+H)+.

According to the analysis of related databases, 5334-39-4, the application of this compound in the production field has become more and more popular.

Adding a certain compound to certain chemical reactions, such as: 18048-64-1, name is 1-(3,4-Dimethylphenyl)-3-methyl-1H-pyrazol-5(4H)-one, 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 18048-64-1, HPLC of Formula: C12H14N2O

Take 11.5g82.4%) of 3′-amino-2′-hydroxybiphenyl-3-formic acid(VI) obtained in step ( 2), (6.8 g, 82.4%) 2-(3,4-dimethylphenyl)-1,2-dihydro-5-methyl-3H-pyrazol-3-one (VII) was added, condensation and cyclization reactions took place, and then Ethanolamine was added under the action of hydrogen to produce the synthesis reaction of Eltrombopag (IX); The 3′-amino-2′ hydroxybiphenyl-3-formic acid and 2-(3,4-dimethylphenyl)-1,2-dihydro-5-methyl-3H-pyrazole- 3-one(VII) in step (3), reacted in a mixed solution of sodium nitrate and sodium bicarbonate.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-(3,4-Dimethylphenyl)-3-methyl-1H-pyrazol-5(4H)-one, and friends who are interested can also refer to it.

Application of 2458-26-6,Some common heterocyclic compound, 2458-26-6, name is 3-Phenyl-1H-pyrazole, molecular formula is C9H8N2, 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 0 C, a solution of 3-phenyl-1H-pyrazole (0.61 g, 5.3 mmol) in dry THF (10 mL) was added dropwise to a suspension of NaH (0.13 g,5.34 mmol) in dry THF (10 mL). After 15 min of stirring, a solution of 2,6-pyridine-dimethylene-ditosylate (1.20 g, 2.67 mmol) in dry THF (15 mL) was added to this solution; the mixture was stirred overnight and filtered, and the solvent was removed. The crude product was purified by column chromatography on silica gel with hexane:EA = 1:1 as eluent to afford 0.41 g (40%) of pure ligand as a white oil that solidified with time. Single crystals were obtained by slow diffusion of hexane into a concentrated solution of the ligand in THF at room temperature. 1H NMR (300 MHz, acetone-d6): 7.84(m, 2H, 4H, 5-H Pz, 2,6-H Ph), 7.65 (t, J = 7.8 Hz, 1H, 4-H Py), 7.36(t, J = 7.2 Hz, 4H, 3,5-H Ph), 7.26 (t, J = 7.5 Hz, 2H, 4-H Ph), 6.96 (d,J = 7.8 Hz, 2H, 3,5-H Py), 6.72 (d, J = 2.4 Hz, 2H, 4-H Pz), and 5.48 (s,4H, PyCH2Pz).13C NMR (75 MHz, acetone-d6): 157.9 (2C, 2,6-CPy), 152.2 (2C, 3-C Pz), 138.9 (1C, 4-C Py), 134.8 (2C, 1-C Ph), 132.9(2C, 5-C Pz), 129.3(4C, 3,5-C Ph), 128.2 (2C, 4-C Ph), 126.1 (4C, 2,6-CPh), 121.2 (2C, 3,5-C Py), 103.7 (2C, 4-C Pz), and 57.9 (2C, PyCH2Pz).

The synthetic route of 2458-26-6 has been constantly updated, and we look forward to future research findings.

Synthetic Route of 37718-11-9, These common heterocyclic compound, 37718-11-9, name is 1H-Pyrazole-4-carboxylic acid, 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 suspension of lH-pyrazole-4-carboxylic acid (50 g, 446 mmol) in 500 ml DMF was added p-toluenesulfonic acid(8.48 g, 44 mmol) and DHP (132 mL, 1561 mmol).The reaction medium turned yellow and then changed at room temperature for 20 hoursblack. The reaction mixture was poured into saturated aqueous NaHCO3 and extracted with EtOAc. The aqueous phase was added by the addition of 6M hydrochloric acid solutionTo pH = 3. The resulting precipitate was filtered off and washed with water and then dried in vacuo at 50 C to give 61.2 g of a white powder(Yield: 70%).

The synthetic route of 37718-11-9 has been constantly updated, and we look forward to future research findings.

Electric Literature of 2075-46-9,Some common heterocyclic compound, 2075-46-9, name is 4-Nitro-1H-pyrazole, molecular formula is C3H3N3O2, 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 solution of 4-nitro-lH-pyrazole (1.13 g, 10.0 mmol) and iodomethane (1.25 mL, 20.0 mmol) in DMF (12 mL), NaH (60% in mineral oil, 0.600 g, 15.0 mmol) was added. The mixture was stirred for 18 h. Water and EtOAc were added. The organic phase was separated, washed with water, dried over Na2S04, concentrated in vacuo to give l-methyl-4- nitro-lH-pyrazole as a solid (1.11 g).

The synthetic route of 2075-46-9 has been constantly updated, and we look forward to future research findings.