Day: November 16, 2020

176969-34-9,Some common heterocyclic compound, 176969-34-9, name is 3-(Difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid, molecular formula is C6H6F2N2O2, 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: Under nitrogen atmosphere, carboxylic acid II (3mmol), EDCI (3.3 mmol), HOBT (3.3 mmol)and Et3N (1.8 mmol) were placed in a three-necked flask with 40 mL CH2Cl2, and stirred for 2 hat 0 C; then, compound I (2.4 mmol) was added to the flask and allowed to react for 3 h at 0 C.The reaction was monitored by thin-layer chromatography (TLC) (all reactions could be completed in3 h) and, on completion of the reaction, the mixture was washed with saturated NaHCO3 solutionand water, respectively. Then, it was dried over anhydrous Na2SO4, filtered and evaporated onrotavapor in vacuum. Subsequently, crude products III-1-III-18 were purified by silica gel columnchromatography [V (CH2Cl2): V (EA) = 3:1] and crude products III-19-III-36 were purified by silicagel column chromatography [V (PE): V (EA) = 3:1]. Finally, products were recrystallized with thedichloromethane/petroleum ether to obtain pure target compounds.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3-(Difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid, its application will become more common.

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 31037-02-2 as follows. 31037-02-2

The ligand, L (0.169 g; 1 mmol), was dissolved in hot MeOH (5 cm3), and CuCl2¡¤2H2O (0.085 g; 0.5 mmol) was added. Afew hours later, the brown microcrystals were filtered andwashed with MeOH and Et2O.Yield: 0.143 g (61%). Calcd. (Found) for CuC14H22N6Cl2: C, 35.56; H, 4.65; N, 17.78; (C,35.42; H, 4.64; N, 17.75). IR bands [ v/cm-1]: 3489, 3440,3347, 1682, 1633, 1557, 1460, 1218, 773. Molar conductivity,LambdaM (S cm2 mol-1): 24 (DMF).

According to the analysis of related databases, 31037-02-2, the application of this compound in the production field has become more and more popular.

The chemical industry reduces the impact on the environment during synthesis 288-13-1, name is 1H-Pyrazole, I believe this compound will play a more active role in future production and life. 288-13-1

Following General Procedure A (90 0C, 30 hours), 1H-pyrazole (205 mg, 3.0 mmol) is coupled with 1-(4-bromophenyl)ethanone (398 mg, 2.0 mmol). The crude brown oil is purified by flash chromatography on silica gel (eluent: dichloromethane/hexanes = 50/50) to provide 300 mg (81 % isolated yield) of the desired product as a white solid. IdentificationMp: 108 JOC.1H NMR (400 MHz, CDCI3): delta 7.98-8.00 (m, 3H, H3|5,7), 7.70-7.76 (m, 3H, H2>6.9), 6.46 (s, 1H, H8), 2.56 (s, 3H, H11).13C NMR (100 MHz, CDCI3): delta 196.84 (C10), 143.33 (C1), 142.09 (C9), 134.80 (C4), 130.01 (C3,beta), 126.91 (C7), 118.39 (C216), 108.62 (C8), 26.60 (C11).IR (KBr) : v (crrf1) = 3135, 3114, 3101 , 1673(C=O), 1605, 1528, 1395, 1264,1210, 935, 838, 762, 611 , 589, 518.GC/MS: rt = 19.96 min, M/Z = 186.HRMS: 187.0893 (M+H). Theoretical: 187.0871.

The chemical industry reduces the impact on the environment during synthesis 288-13-1. I believe this compound will play a more active role in future production and life.

A common heterocyclic compound, 35277-02-2, name is 4-Fluoro-1H-pyrazole, molecular formula is C3H3FN2, 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. 35277-02-2.

A mixture of tert-butyl 4-[[2-[5-bromo-3-(methoxymethoxy)-2-pyridyl]thiazolo[5,4-d]thiazol-5- yl]-methyl-amino]piperidine-l-carboxylate (86 mg, 0.15 mmol), obtained using the chemistry described in Example 16, Step 2, 4-fluoro-lH-pyrazole (19 mg, 0.22 mmol), cuprous iodide (3 mg, 0.016 mmol), trans-N,N’-dimethylcyclohexane-l, 2-diamine (5 mg, 0.034 mmol) and K2CO3 (52 mg, 0.38 mmol) in toluene (0.3 mL) was stirred at 100 C for 12 h. The reaction was concentrated, diluted with CH2CI2 and washed with aqueous NH4CI, brine and dried. After the removal of the solvent, the residue was chromatographed (EtOAc in CH2CI2, 0-100%) to provide tert-butyl 4- [ [2- [5-(4-fluoropyrazol- 1 -yl)-3 -(methoxymethoxy)-2-pyridyl] thiazolo [5 ,4-d] thiazol- 5-yl]-methyl-amino]piperidine-l-carboxylate. The product was treated with HC1 in dioxane (3.0 mL, 4.0 M) at room temperature for 4 h and the precipitate was collected, wahsed with diethyl ether and dried to provide 5-(4-fluoropyrazol-l-yl)-2-[5-[methyl(4-piperidyl)amino]thiazolo[5,4- d]thiazol-2-yl]pyridin-3-ol hydrochloride (46 mg, 65.2%). LC-MS 432.4 [M+H]+, RT 1.21 min, 1H NMR (DMSO -d6) d: 11.15 (br s, 1H), 8.69-8.94 (m, 3H), 8.65 (d, 7=2.1 Hz, 1H), 7.97 (d, 7=4.0 Hz, 1H), 7.86 (d, 7=2.1 Hz, 1H), 4.37-4.62 (m, 1H), 3.33- 3.42 (m, 2H), 3.04-3.19 (m, 2H), 3.01 (s, 3H), 2.03-2.18 (m, 2H), 1.84-1.97 (m, 2H).

The synthetic route of 4-Fluoro-1H-pyrazole has been constantly updated, and we look forward to future research findings.

83-10-3, 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. 83-10-3 name is 1,5-Dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazole-4-carboxylic acid, 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.

Step 2) N-(2-fluoro-4-hvdroxyphenyl)-L5-dimethyl-3-oxo-2-phenyl-2,3-dihvdro-lH- pyrazole-4-carboxamide [0205] To a suspension of 4-amino-3-fluorophenol (1.0 g, 7.87 mmol) and 1,5- dimethyl-3-oxo-2-phenyl-2,3-dihydro-lH-pyrazole-4-carboxylic acid (2.19 g, 9.44 mmol) in CH2C12 (20 mL) were added EDCI (3.02 g, 15.7 mmol) and HOAT (0.21 g, 1.57 mmol). The reaction mixture was refluxed for 20 hours, and then cooled to rt. Water (10 mL) was added and the mixture stirred at rt overnight, then filtered and the filter cake was washed with water (5 mL), followed by purifying by a silica gel column chromatography (CH2Cl2/MeOH (v/v) = 70/1) to give the title compound as a beige white solid (1.25 g, 46.6%). MS (ESI, pos, ion) m/z: 342.1 [M+H]+, Rt = 2.712 min.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,5-Dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazole-4-carboxylic acid, and friends who are interested can also refer to it.

The chemical industry reduces the impact on the environment during synthesis 176969-34-9, name is 3-(Difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid, I believe this compound will play a more active role in future production and life. 176969-34-9

3 -(difluorochloromethyl)-l -methyl- lH-pyrazol-4-carboxylic acid obtained by example 5 is treated with oxalyl chloride (1,25 eq) in toluene, and a few drops of dimethylformamide are added. The mixture is concentrated under reduced pressure to yield the carboxyl chloride.

The chemical industry reduces the impact on the environment during synthesis 176969-34-9. I believe this compound will play a more active role in future production and life.

25222-43-9, 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. 25222-43-9, name is (1H-Pyrazol-4-yl)methanol, A new synthetic method of this compound is introduced below.

(11H-Pyrazol-4-yl) methanol was Boc-protected by reaction with Boc-anhydride (1 .2 eq) and triethylamine (2.5 eq) in DCM at 0 ¡ãC, with warming to ambient temperature. The alcohol of this Boc-protected amine was then converted to the mesylate by reaction with methanesulfonyl chloride (1 .5 eq) and triethylamine (2.5 eq) in DCM at 0 ¡ãC, with warming to ambient temperature for 2 h. N-[1 -(Fluoromethyl)cyclopropyl]-3-[(1 -methylpyrazol-4- yl)methyl]-2,4-dioxo-1 H-quinazoline-6-sulfonamide (100 mg, 0.260 mmol), the mesylate (79 mg, 0.286 mmol) and potassium carbonate (54 mg, 0.39 mmol) in DMF was conventionally heated to 70 ¡ãC for 4 h. After Boc-deprotection with HCI in dioxane, usual work-up afforded the desired product (14 mg, 0.029 mmol, 1 1 percent) as a white powder.

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.

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. 1453-58-3, name is 3-Methylpyrazole, A new synthetic method of this compound is introduced below., 1453-58-3

10298] To a solution of 3-methyl-1H-pyrazole (10.99 g, 134 mmol) in N,N-dimethylformamide (100 ml) at 0¡ã C. was added sodium hydride (3.71 g, 154 mmol, 60percent dispersion). The reaction was stirred at 0¡ãC. for2 hours. 3-Fluoropyridine (10.0 g, 103 mmol) was added, and the reaction was stirred at 100¡ã C. overnight. The reaction was cooled to room temperature and water was added slowly. The mixture was extracted with dichloromethane and the combined organic phases were washed with brine, concentrated and chromatographed (0-100percent ethyl acetate/hexanes) to afford 3-(3-methyl-1H- pyrazol-1-yl)pyridine (8.4 g, 52.77 mmol, 5 1.2percent) and 3-(5- methyl-i H-pyrazol- 1 -yl)pyridine (1.0 g, 6percent). Analytical data of both products is consistent with that reported under Example 6, Step 1.

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.

1192-21-8, 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.

[00180] Step 3: To a solution of dioxane (150 mL) was added 2-chloro-4-(2- fluoropyridin-4-yl)pyrimidine (15.0 g, 72.1 mmol), 1 -methyl- lH-pyrazol-5 -amine (7.6 g, 79.3 mmol), cesium carbonate (35.3 g, 108.0 mmol), Pd2(dba)3 (6.6 g, 7.2 mmol) and xantphos (8.3 g, 14.4 mmol). The mixture was heated at 80 ¡ãC under a nitrogen atmosphere for 2 hours. TLC (PE:EtOAc = 5: 1) indicated that the starting material was consumed. The mixture was cooled to room temperature and filtered through a bed of Celite?. The filtrate was then partitioned between EtOAc (200 mL) and water (100 mL). After separation, the organic layer was washed with water, brine, dried over anhydrous MgS04, filtered, concentrated and then purified by column chromatography on silica gel (PErEtOAc = 10: 1 to about 1 : 1) to provide 4-(2-fluoropyridin-4-yl)-N-(l -methyl- lH-pyrazol-5-yl)pyrimidin-2- amine (14.5 g, 74percent) as a solid.

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.

1621-91-6, 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. 1621-91-6, name is 1H-Pyrazole-3-carboxylic acid, A new synthetic method of this compound is introduced below.

Sulfuric acid (5.8 mL) was added dropwise to a stirred solution of 1H-pyrazole-3-carboxylic acid (1 g, 8.92 mmol) in MeOH (65 mL) at 0 C. After the addition was completed the mixture was allowed to warm to room temperature and stirred for 18 hours. The mixture was concentrated in vacuo and the residue was dissolved in water and basified with NaHCO3 (aq. sat. solution). The mixture was extracted with AcOEt. The organic layer was separated, dried (MgSO4), filtered and the solvents evaporated in vacuo to yield 1H-pyrazole-3-carboxylic acid methyl ester (0.7 g, 62% yield) as a white solid which was used in the next step without further purification.

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.