Tag: M.W:100-200

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. 2075-46-9, name is 4-Nitro-1H-pyrazole belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below. 2075-46-9

General procedure: A mixture of methyliodide (12 mmol), 1a (6 mmol) and K2CO3 (9 mmol) in DMF (6 mL) was stirred overnight at room temperature. Then the reaction mixture was diluted with water (20 mL) and extracted with ethyl acetate (25 mL ¡Á 3). The organic layer was washed with aqueous saturated sodium bicarbonate, dried by sodium sulfate, ltered and concentrated in vacuum. Purication by ash column chromatography gave the desired product 2a (2a-2c).A mixture of iodobenzene (6.82 mmol), 1a (0.70 g, 6.20 mmol), 8-hydroxyquinoline (0.09 g, 0.62 mmol), cuprous iodide (0.18 g, 0.62 mmol) and potassium carbonate (1.73 g, 12.40 mmol) in DMSO (10 mL) was heated at 135 oC for 20 h. After cooling to room temperature, the reaction mixture was diluted with water (20 mL) and extracted with ethyl acetate. The organic layer was washed with aqueous saturated sodium bicarbonate, dried by sodium sulfate, filtered and concentrated in vacuo. Purification by flash column chromatography gave the desired products 2d (2d-2g).

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

15366-34-4, A common compound: 15366-34-4, name is Methyl 1H-pyrazole-3-carboxylate, belongs to pyrazoles-derivatives compound, it can change the direction of chemical reaction, and react with certain compounds to generate new functional products. A new synthetic method of this compound is introduced below.

Methyl 1H-pyrazole-3-carboxylate (0.500 g, 3.96 mmol), was dissolved in DCE (25 mL), then cyclopropylboronic acid (0.681 g, 7.93 mmol) and sodium carbonate(0.840 g, 7.93 mmol) were added. The reaction mixture was heated to 70 C, and then a mixture of 2,2?-bipyridine (0.6 19 g, 3.96 mmol) and copper(II) acetate (0.720 g, 3.96 mmol) were added in one batch. The reaction mixture was stirred at 70 C under oxygen atmosphere (1 atm) for 2 d. Saturated aq. NaHCO3 solution was added to the reaction mixture, and it was extracted with EtOAc (3x). The combined organic phase was concentrated. The residue was purified by flash chromatography (solid loading on CELITE, 0-65% EtOAc/Hex) affording two products.Intermediate 15A (0.119 g, 18% yield) as a colorless syrup eluted at 2O% EtOAc. MS(ESI) m/z: 167.0 (M+H) ?H NMR: (400 MHz, DMSO-d6) oe ppm 7.40 (d,J=2.0 Hz, 1H), 6.82 (d, J=2.0 Hz, 1H), 4.31 -4.24 (m, 1H), 2.11 (s, 3H), 1.29- 1.22 (m,2H), 1.10- 1.00 (m, 2H).Intermediate 16A (0.37 1 g, 56% yield) as a colorless syrup eluted at 45% EtOAc. MS(ESI) m/z: 167.0 (M+H) ?H NMR: (400 MHz, DMSO-d6) oe ppm 77.46 (d, J=2.4 Hz, 1H), 6.78 (d, J=2.2 Hz, 1H), 3.92 (s, 3H), 3.67 (tt, J=7.4, 3.9 Hz, 1H), 1.23 -1.15 (m, 2H), 1.09- 1.01 (m, 2H).

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

1621-91-6,Some common heterocyclic compound, 1621-91-6, name is 1H-Pyrazole-3-carboxylic acid, molecular formula is C4H4N2O2, 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: Into a 1L open reactor was added 500g of carboxylic acid raw material (chemically pure) and stirring was turned on (600 r/min) from the reactorThe bottom is continuously fed with ammonia gas (chemical purity, water content of 5.1% by weight, flow rate of 100 g/min) to the carboxylic acid feed. After the reaction was allowed to proceed for TC hours at the reaction temperature TA, ammonia gas flow was stopped. The contents of the reactor were sampled and subjected to nuclear magnetic proton and elemental analysis to characterize the amide intermediate. Specific reaction conditions and characterization results are shown in Table A-1, Table A-2, Table A-3, Table A-4, Table A-5 and Table A-6. These characterization results show that the amide intermediates obtained have an extremely high purity (above 99%).In this embodiment, the ammonia gas can be directly replaced with waste ammonia gas (from Yangzi Petrochemical Plant, containing approximately50wt% of ammonia gas, the rest were toluene, oxygen, nitrogen, steam, carbon monoxide, and carbon dioxide, and the flow rate of this waste ammonia was 130g/min).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1H-Pyrazole-3-carboxylic acid, its application will become more common.

6076-12-6, 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. 6076-12-6, name is Ethyl 4-methyl-1H-pyrazole-3-carboxylate, A new synthetic method of this compound is introduced below.

Compound 258.1. Ethyl 5-iodo-4-methyl-lH-pyrazole-3-carboxylate. Into a 250- mL round-bottom flask, was placed a solution of ethyl 4-methyl-lH-pyrazole-3-carboxylate (600 mg, 3.89 mmol) in N,N-dimethylformamide (20 mL). MS (2.2 g, 9.78 mmol) was added and the resulting mixture was stirred for 6 h at 50 C, then quenched with water (10 mL). The mixture was extracted with ethyl acetate (3 x 40 mL) and the combined organic extracts were washed with aqueous a2S203 (sat., 2 x 30 mL) and brine (2 x 20 mL), dried ( a2S04), filtered and concentrated under reduced pressure. The residue was purified by a silica gel chromatography with ethyl acetate/petroleum ether (1 : 10) as eluent to obtain the title compound as a white solid (800 mg, 73%).

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.

A common heterocyclic compound, 176969-34-9, name is 3-(Difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid, molecular formula is C6H6F2N2O2, 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. 176969-34-9.

3-(difluoromethyl)-1 -methyl-i H-pyrazole-4-car-boxylic acid (2 g, 11.36 mmol) was dissolved in 20 mL sulthryl dichloride, and then heated to reflux for 3 h, the excessive sulfuryl dichloride was evaporated under reduced pressure to get 3-(difluoromethyl)-i -methyl- iH-pyrazole-4- carbonyl chloride, and then the carbonyl chloride was dissolved in 30 mL dichloromethane for the following reaction. To a cooled solution of (3-aminophenyl)methanol (1.4 g, 11.36 mmol) dissolved in 20 mL dichloromethane and 5 mL triethylamine was added slowly the solution of the carbonyl chloride at 0-5 C. Afier the reaction was stirred for 6 h at room temperature, analysis by Thin-Layer Chromatography showed complete conversion to product, the excessive solvent was evaporated under reduced pressure. the residual was purified by column chromatography on silica gel (eluent: ethyl acetate:petroleum ether=i:3; silica gel: 100-140 mesh, Qingdao Marine Chemical Co., Ltd.) to obtain 3-(di- fluoromethyl)-N-(3-(hydroxymethyl)phenyl)- i-methyl-i Hpyrazole-4-carboxamide (2.32 g) as white solid with yield of 73%. ?H NMR (300 MHz, CDC13) oe (ppm): 4.11 (s, 3H),4.73 (s, 2H), 7.16-7.81 (m, 6H).

The synthetic route of 3-(Difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid has been constantly updated, and we look forward to future research findings.

139756-02-8, Adding a certain compound to certain chemical reactions, such as: 139756-02-8, name is 4-Amino-1-methyl-3-N-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 139756-02-8.

Synthesis of Bm; Step 7: 4-amino-i-methyl-3-propyl-iH-pyrazole-5-carboxamide (1 eq) and 2-chlorobenzaldehyde (1.1 eq) were suspended in ethanol 5 ml and the mixture heated at 65 C for 2 hours after conformation of forming of imine by TLC. AddedCuC12 (3 eq) and the reaction mixture heated at 70 C under 02 for 2 hours. After completion of the reaction, the ethanol was removed under vacuum. Then workup with ethyl acetate and water. Separate the organic layer and Water layer re-extracted with 2x25m1 ethyl acetate. The combined organic layers are washed with brine solution, concentrated under vacuum. The residue was purified by column chromatography onsilica the desired product Bm as a white solid; yield 88%. ?H NMR (200 MHz CDC13) oe12.06 (s 1H ),8.0i (M, 1H), 7.45 (m, 1H), 7.32 (td, J= 7.8, 1.5 Hz, 1H), 7.21 (td, J=7.5, 1.4 Hz, 111), 4.05 (s, 3H), 3.03 (t, J= 7.4 Hz, 2H), 1.86 (m, 211), 1.06 (t, J- 7.4 Hz,3H). MASS: ESI [M + H] + : 287.12; Elemental anal. calcd. for C15H15FN40 ; C,62.93; H, 5.28; F, 6.64; N, 19.57; 0, 5.59; found C, 62.88; H, 5.31; F, 6.64; N, 19.57;0,5.61.

According to the analysis of related databases, 139756-02-8, the application of this compound in the production field has become more and more popular.

82560-12-1, name is 3-Amino-5-tert-butylpyrazole, 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. 82560-12-1

c. 2-[5-(5-Amino-3-tert-butyl-pyrazol-1-yl)-2-chloro-phenyl]-ethanol (Intermediate Rc) A suspension of Intermediate Rb (236 mg, 0.835 mmol), 3-tert-butyl-1H-pyrazole-5-amine (Fluorochem, 122 mg, 0.88 mmol), copper(I) iodide (8.00 mg, 0.04 mmol), trans-N,N’-dimethylcyclohexane-1,2-diamine (23.8 mg, 0.17 mmol) and K2CO3 (242 mg, 1.75 mmol) in degassed toluene (1 mL) was stirred at 100 C. under Ar for 3 h, and then heated to 150 C. for 5 h using microwave irradiation. The cooled solution was partitioned between EtOAc (10 mL), water (5 mL) and concentrated aqueous ammonia (5 mL). The aqueous layer was extracted with EtOAc (10 mL), then the combined organics washed with water (10 mL), brine (10 mL), dried (Na2SO4), filtered and concentrated in vacuo to leave a oil (305 mg). FCC, using 20-45% EtOAc in cyclohexane, gave the title compound as an opaque sticky gum (129 mg, 53%). LCMS (Method 3): Rt 2.80 min, m/z 294 [MH+].

Statistics shows that 82560-12-1 is playing an increasingly important role. we look forward to future research findings about 3-Amino-5-tert-butylpyrazole.

15366-34-4,Some common heterocyclic compound, 15366-34-4, name is Methyl 1H-pyrazole-3-carboxylate, molecular formula is C5H6N2O2, 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.

Method 75 Synthesis of methyl 4-[1-[4-(2-aminopyrimidin-5-yl)phenyl]cyclobutyl]-1H-pyrrole-3-carboxylate (Example 162) To a solution of I-66.1 (100 mg, 0.41 mmol) in nitromethane (5 mL) is added iron (III) chloride (20.16 mg, 0.12 mmol) and methyl-1H-pyrazole-3-carboxylate (62.2 mg, 0.497 mmol) and is stirred at room temperature for 24 hours. The reaction is concentrated in vacuo, and the residue is partitioned between saturated aqueous NaHCO3 and EtOAc. The combined organics are dried with Mg2SO4, filtered, and concentrated in vacuo. The residue is purified by flash chromatography (SiO2, 0-10% MeOH in CH2Cl2) to give the title compound 162 (5 mg).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Methyl 1H-pyrazole-3-carboxylate, its application will become more common.

2075-46-9, 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. 2075-46-9 name is 4-Nitro-1H-pyrazole, 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.

General procedure: To a stirred solution of 4-nitro-1H-pyrazole (2 g, 17.7 mmol) inacetonitrile (15 mL) was added potassium carbonate (2.7 g, 19.5 mmol)and iodomethane (2.76 g, 19.5 mmol). The reaction mixture was stirredat reflux temperature for 6 h. And it was evaporated to dryness. Thecrude mass was purified by silica gel column chromatography (PE:EA=10:1) to afford compound 15c (2.2 g, 98%) as a white solid. MS(ESI) m/z 128 [M+H]+.

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

2075-46-9, 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. 2075-46-9, name is 4-Nitro-1H-pyrazole, This compound has unique chemical properties. The synthetic route is as follows.

4-Nitropyrazole (2.0 g, 17.68 mmol),The solution obtained by dissolving 2-chloroethyl methyl ether (2.01 g, 21.26 mmol) and potassium carbonate (4.88 g, 35.31 mmol) in 40 mL of acetonitrile was refluxed for 18 h.Spin dry,A silica gel column (PE/EA = 4:1) gave 1.5 g of a pale yellow solid.Yield: 49.5%.

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.