Day: April 20, 2021

Electric Literature of 139308-52-4,Some common heterocyclic compound, 139308-52-4, name is Ethyl 3-bromo-1-methyl-1H-pyrazole-4-carboxylate, molecular formula is C7H9BrN2O2, 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.

The reaction mixture of ethyl 3-bromo-1-methyl-pyrazole-4-carboxylate (200 mg, 0.86 mmol), 4-methoxypiperidine (197.67 mg, 1.72 mmol), Cs2CO3 (838.79 mg, 2.57 mmol) and XtanTphos Pd G3 (162.76 mg, 0.17 mmol) in dimethylacetamide (5 mL) was heated at 120 C. overnight. The reaction mixture was cooled down, washed with water, extracted with EtOAc, dried over MgSO4, filtered, concentrated, and purified by silica gel chromatography (0-100% EtOAc/hexane) to give the product (14 mg).

The synthetic route of 139308-52-4 has been constantly updated, and we look forward to future research findings.

These common heterocyclic compound, 1613191-73-3, name is Allyl 3,5-diamino-1H-pyrazole-4-carboxylate, 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. COA of Formula: C7H10N4O2

Preparation 2a: lH-benzo[d] [l,2,3]triazol-l-yl 2-amino-6-fluoropyrazolo[l,5- a] pyrimidine-3-carboxylate 6a Step 1: allyl 2-amino-6-fluoro-pyrazolo [ 1 ,5-a] pyrimidine-3-carboxylate 4a [00244] To a suspension of allyl 3,5-diamino-lH-pyrazole-4-carboxylate 3 (42.72 g, 234.5 mmol) in DMSO (270.8 mL) / Water (270.8 mL), was added p-TsOH hydrate (46.72 g, 245.6 mmol) and 3-(diisopropylamino)-2-fluoro-prop-2-enal (described in Tetrahedron Letters, 33(3), 357-60; 1992) (38.69 g, 223.3 mmol). The reaction mixture was heated to 100C for 3h during which time a solid slowly precipitated out of solution. The orange suspension was allowed to cool down to RT overnight. The solid was filtered, washed with water and dried under vacuum to give allyl 2-amino-6-fluoro-pyrazolo[l,5-a]pyrimidine-3-carboxylate 4a as a sand solid (45.05 g, 85% yield).

The synthetic route of Allyl 3,5-diamino-1H-pyrazole-4-carboxylate has been constantly updated, and we look forward to future research findings.

Application of 2458-26-6, 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. 2458-26-6 name is 3-Phenyl-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: In an oven-dried vial equipped with a magnetic stirrer and a PTFE septum, [Ir{dF(CF3)ppy}2](dtbpy)]PF6 (5.6 mg, 1 mol%) was added to a mixture of the substrate (0.5 mmol, 1 equiv), CF3SO2Na (1.5 mmol, 3 equiv), and (NH4)2S2O8 (0.5 mmol, 1 equiv) in DMSO (5 mL). The solution was pumped into the Vapourtec photoreactor (fluoropolymer tube, 1.3 mm i.d., 10 mL) and the liquid flowrate was set at 0.33 mL/min (30 min residence time). The reactor was irradiated with 54 blue LEDs (450 nm, total power 24 W). The reaction mixture collected from the outlet was diluted with H2O and extracted with Et2O (3¡Á). The combined organic layers were washed with brine, dried over MgSO4, and concentrated in vacuo. The crude was then pre-adsorbed onto silica, dried in vacuo, and purified by flash chromatography to yield the trifluoromethylated product.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3-Phenyl-1H-pyrazole, and friends who are interested can also refer to it.

26308-42-9, name is 3-Ethyl-1-methyl-1H-pyrazole-5-carboxylic acid, 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. Recommanded Product: 26308-42-9

General procedure: 3a (0.01 mol) and thionyl chloride (2.95 g, 0.025 mol) were successively added to 15 ml 1,2-dichloroethane. After 2 h under reflux, the solvent was removed under reduced pressure. 4a was obtained and without further purification and calculating the yield, next reaction was carried out immediately. The analogues 4b-p were prepared in a similar procedure.

The synthetic route of 26308-42-9 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. 121507-34-4, name is 5-Isopropoxy-1H-pyrazol-3-amine, A new synthetic method of this compound is introduced below., name: 5-Isopropoxy-1H-pyrazol-3-amine

Example 68; N’-(5-isopropoxy-1H-pyrazol-3-yl)-6-methyl-N-[(3-methylisoxazol-5-yl)methyl]pyrimidine-2,4-diamine (also known as 6-methyl-N-[(3-methyl-1,2-oxazol-5-yl)methyl]-N’-(5-propan-2-yloxy-1H-pyrazol-3-yl)pyrimidine-2,4-diamine)A mixture of 4-chloro-6-methyl-N-[(3-methylisoxazol-5-yl)methyl]pyrimidin-2-amine (also known as 4-chloro-6-methyl-N-[(3-methyl-1,2-oxazol-5-yl)methyl]pyrimidin-2-amine; 0.20 g, 0.84 mmol) and 5-isopropoxy-1H-pyrazol-3-amine (0.178 g, 1.26 mmol) in anhydrous 1-methylpyrrolidinone (2 mL) and 4M hydrogen chloride solution in dioxane (0.42 mL) was heated at 110 C. for 4 hours. The mixture was left to stand at room temperature overnight and was then diluted with saturated sodium bicarbonate solution and extracted with ethyl acetate (¡Á2). The organic extracts were washed with brine, dried over magnesium sulfate, filtered and then evaporated to leave an orange oil. The oil was purified by chromatography on silica eluting with a mixture of 2-4% methanol in dichloromethane. Fractions containing product were combined and then evaporated to leave a solid which was triturated with diethyl ether to leave example 68 in table 4 (0.039 g, 12% yield).1H NMR (500 MHz, DMSO at 373K): 1.28 (d, 6H), 2.15 (s, 3H), 2.19 (s, 3H), 4.58 (d, 2H), 4.64 (bs, 1H), 5.25 (bs, 1H), 5.41 (bs, 1H), 6.12 (s, 1H), 7.2 (bs, 1H), 9.33 (bs, 1H), 11.39 (bs, 1H).MS: m/z 344 (MH+).

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.

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. 578008-32-9, name is tert-Butyl 3-amino-5-methyl-1H-pyrazole-1-carboxylate, This compound has unique chemical properties. The synthetic route is as follows., name: tert-Butyl 3-amino-5-methyl-1H-pyrazole-1-carboxylate

2,6-Dichloropyrazine (5.0 g, 33.6 mmol), tert-butyl 3-amino-5-methyl-lH- pyrazole-1-carboxylate (6.62 g, 33.6 mmol), palladium(II) acetate (0.75 g, 3.36 mmol), 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (3.88 g, 6.71 mmol), potassium carbonate (46.4 g, 336 mmol), and dioxane (224 mL) were combined and the mixture was degassed with nitrogen for 2 minutes before heating to 90C for one hour. The reaction was cooled to room temperature and filtered through Celite followed by washing with dichloromethane. The filtrate was condensed and the crude material was purified by silica gel chromatography (10-70% ethyl acetate in hexanes) to give the title compound as a white solid (6.43 g, 20.8 mmol, 62% yield); MS (ESI) MS (ESI) m/z 310.5 [M+l]+.

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 578008-32-9.

Electric Literature of 39806-90-1, 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 39806-90-1 as follows.

1-Methyl-4-((trimethylsilyl)ethynyl)-1H-pyrazole (19) 1-Methyl-4-iodo-pyrazole (18) (5.0 g 24.04 mmole) was dissolved in DMF (32 mL) and ethynyltrimethylsilane (4.76 mL, 3.31 g, 33.7 mmole) was added followed by diisopropylamine (4.46 mL, 3.21 g 31.78 mmole), copper(I) iodide (304 mg 1.59 mmole) and triphenylphosphine (1.26 g 4.81 mmole). The reaction was flushed with argon. Palladium acetate (351 mg 1.56 mmole) was added and the reaction was again flushed with argon. It was heated at 60 C. for 60 mins. The reaction was cooled, added to water (350 ml) and extracted with ether (3*100 mL). The organic solution was filtered from a brown solid which was washed with a little more ether. The organic solution was washed with water (3*80 mL), brine, dried and evaporated. The crude product was flash chromatographed (silica) using 1:4 ethyl acetate:cyclohexane and then 1:3 ethyl acetate:cyclohexane to give the title compound as a solid (2.85 g 67%). 1H-NMR (CDCl3, 500 MHz): delta 0.24 (s, 9H), 3.87 (s, 3H), 7.50 (s, 1H), 7.58 (s, 1H).

According to the analysis of related databases, 39806-90-1, 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. 37687-26-6, name is Diethyl 1H-pyrazole-3,4-dicarboxylate belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below. Product Details of 37687-26-6

To a stirred solution of 104B (19 g, 90 mmol) in DMF (50 mL) was added NIS (30.2 g, 134 mmol) and the reaction mixture was stirred for 16 h at 115 C. LCMS indicated the completion of the reaction. DMF was evaporated, the crude was dissolved in EtOAc, washed with water, sodium thiosulfate solution, dried, filtered and evaporated under vacuum to furnish crude product, which was purified by ISCO using EtOAc and hexane system. Fractions collected at 18-20% EtOAc in hexane were evaporated to get 104C (12.5 g, 37.0 mmol, 41.3% yield). MS(ES): m/z=338 [M+H]+; 1H NMR (400 MHz, DMSO-d6) delta ppm 14.25 (bs, 1H), 4.27 (m, 4H), 1.26 (m, 6H).

The synthetic route of 37687-26-6 has been constantly updated, and we look forward to future research findings.

Electric Literature of 39806-90-1,Some common heterocyclic compound, 39806-90-1, name is 4-Iodo-1-methyl-1H-pyrazole, molecular formula is C4H5IN2, 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.

A solution of 4-iodo-1-methyl-1H-pyrazole (83.8 mg, 0.403 mmol) in THF (0.8 mL) was added dropwise under argon to a -72 C. solution of n-BuLi (0.156 mL, 0.403 mmol, 2.6 M in hexane) in THF (0.5 mL). The resulting mixture was stirred at -72 C. for 25 minutes, and was then treated dropwise with a solution of an inseparable mixture of (3-benzyl-2,4-dichloroquinolin-6-yl)(4-chlorophenyl)methanone (79 mg, 0.185 mmol, Intermediate 33: step d) and ethyl 3-benzyl-2,4-dichloroquinoline-6-carboxylate (66 mg, 0.183 mmol, Intermediate 33: step c) in THF (0.8 mL) and stirred at -72 C. for 30 minutes. The yellow reaction was then allowed to warm to 0 C. over 15 minutes and stirred for an additional 15 minutes at 0 C. The clear amber reaction was then quenched with 5 M aqueous NH4Cl (3 mL). The aqueous layer was extracted with 4:1 ether/DCM (2*3 mL), and the combined organic layers were dried (Na2SO4), filtered, and concentrated. The residue was flash chromatographed with a heptane to 20% EtOAc/heptane gradient and further purified with C18 HPLC (20% to 100% CH3CN, with 0.1% TFA throughout) to provide, after lyophilization, the title compound as a yellow powder. 1H NMR (400 MHz, CDCl3) delta ppm 8.33 (d, J=1.96 Hz, 1H), 7.99 (d, J=8.80 Hz, 1H), 7.69 (dd, J=1.96, 8.80 Hz, 1H), 7.48 (s, 1H), 7.31-7.38 (m, 4H), 7.16-7.31 (m, 6H), 4.53 (s, 2H), 3.96 (s, 3H); MS m/e 507.7 [M+H]+.

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

Related Products of 26621-44-3, The chemical industry reduces the impact on the environment during synthesis 26621-44-3, name is 3-Nitro-1H-pyrazole, I believe this compound will play a more active role in future production and life.

[322] To a 0 C solution of 3-nitro-1H-pyrazole (1.0 g, 8.84 mmol) in NMP (10.0 mL) was added NaH (425 mg of 60 %w/w, 10.63 mmol). After 20 minutes, the mixture was warmed to room temperature and stirred a further 60 minutes. The mixture was re-cooled to 0 C and 2-fluoropyrimidine (1.0 g, 10.20 mmol) was added. The resultant mixture was heated to 80C for 16 h. The reaction mixture was poured over ice, resulting in precipitation of a solid. The product was collected by vacuum filtration, and the solids air-dried to provide 2-(3-nitro-1H-pyrazol-1-yl)pyrimidine (1.66 g, 96% yield). 1H NMR (400 MHz, DMSO-d6) delta 9.00 (d, J = 4.8 Hz, 2H), 8.91 (d, J = 2.9 Hz, 1H), 7.68 (t, J = 4.9 Hz, 1H), 7.35 (d, J = 2.8 Hz, 1H) ppm. ESI-MS m/z calc. 191.04, found 191.96 (M+1).

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