Category: 1254073-41-0

The major producers of chemicals have been the Europe, Japan and China. Due to the growing call for a cleaner, greener environment, people will have to find innovative ways to maintain their relevance. Here is a compound 1254073-41-0, name is 5-Fluoropicolinohydrazide. This compound has unique chemical properties. The synthetic route is as follows. Recommanded Product: 5-Fluoropicolinohydrazide

To a solution of 4-[(2,4-dichloro-3-fluorophenyl)carbonyl]-2-piperazinone (137) (0.146 g, 0.5 mmol) in Dichloromethane (DCM) (3 ml.) was added triethyloxonium tetrafluoroborate (0.100 g, 0.525 mmol). The solution was then stirred, under argon, for 10 minutes before 5-fluoro-2-pyridinecarbohydrazide (I24) (0.093 g, 0.600 mmol) was added. The solution was then stirred for a further hour before the solvent was concentrated and n-butanol (3.00 ml.) was added. The solution was then stirred, under argon and reflux, for 3 hours before being cooled to room temperature. The solvent was then evaporated in vacuo and the remaining residue was purified by flash chromatography (Biotage SP4, 25M cartridge) with a gradient of 0-10% 2M NH3/MeOH in DCM. TLC confirmed product location and the solvent from the combined fractions was evaporated in vacuo. The remaining residue was then further purified by mass-direct automated HPLC, and the solvent evaporated in vacuo. The remaining solid was then triturated with ether and dried in a vac-oven to yield the product in 0.045 g. LCMS: m/z = 409 (M+ H)+, retention time = 0.93 minutes (2 minutes)

With the rapid development of chemical substances, we look forward to future research findings about 1254073-41-0.

Reference:
Patent; GLAXO GROUP LIMITED; DEAN, David Kenneth; MUNOZ-MURIEDAS, Jorge; SIME, Mairi; STEADMAN, Jon Graham Anthony; THEWLIS, Rachel Elizabeth Anne; TRANI, Giancarlo; WALTER, Daryl Simon; WO2010/125102; (2010); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Electric Literature of 1254073-41-0, 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. 1254073-41-0, name is 5-Fluoropicolinohydrazide. A new synthetic method of this compound is introduced below.

Into a solution of 5-fluoropyridine-2-carbohydrazide (1 g) in dichloromethane (30 mL) was mixed triethylamine (2.7 mL), and methyl chloroglyoxylate (0.59 mL) was added thereto under ice-cooling, followed by stirring at room temperature for 5 hours. p-Toluenesulfonyl chloride (1.23 g) was added thereto under ice-cooling, followed by stirring at room temperature overnight. To the reaction mixture was added water at room temperature to carry out liquid separation, and the organic layer was concentrated. After concentration, the obtained oily substance was dissolved in ethyl acetate. Together with the aqueous layer, liquid separation was carried out. The organic layer was washed with a saturated aqueous sodium hydrogen carbonate solution and saturated brine. The organic layer was dried over anhydrous magnesium sulfate, filtered, and concentrated. The obtained solid was collected by filtration while washing with a solvent (hexane:ethyl acetate=4:1) to obtain methyl 5-(5-fluoropyridin-2-yl)-1,3,4-oxadiazole-2-carboxylate (1.073 g) as a gray solid.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,1254073-41-0, its application will become more common.

Reference:
Patent; Astellas Pharma Inc.; EP2511265; (2012); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Synthetic Route of 1254073-41-0, 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. 1254073-41-0, name is 5-Fluoropicolinohydrazide. A new synthetic method of this compound is introduced below.

To a solution of 4-[(2,3-dichloro-4-fluorophenyl)carbonyl]-2-piperazinone (I34) (5.08 g, 17.45 mmol) in Dichloromethane (DCM) (80 mL) was added triethyloxonium tetrafluoroborate (3.48 g, 18.32 mmol). The solution was then stirred under argon for 20 minutes before 5-fluoro-2-pyridinecarbohydrazide (I24) (3.25 g, 20.94 mmol) was added. The solution was then stirred for a further 3 hours, before the solvent was concentrated and n-butanol (80 mL) was added. The solution was then stirred, under reflux and argon, for 3 hours before being cooled to room temperature. The solvent was then evaporated in vacuo and the remaining residue was partioned between DCM (10OmL) and water (5OmL), before being dried over anhydrous sodium suphate. The sodium sulphate was then removed by filtration, and the solvent was evaporated in vacuo. The remaining residue was then purified by flash chromatography (Isolera 34Og cartridge) with a gradient of 0-10% MeOH in DCM, TLC confirmed product location and the solvent from the combined fractions was evaporated in vacuo. The remaining solid was then recrystallised from ethyl acetate to yield the product in 2.067 g.LCMS: m/z = 410 (M+ H)+, retention time = 0.93 minutes (2 minutes); 1H NMR (400 MHz; CDCI3) delta 8.50 ( 0.6H, d), 8.43 – 8.35 ( 1.4H, m), 7.6- 7.54 ( 1 H, m), 7.31-7.19 ( 2H,m), 5.26 ( 1 H, q), 4.82-4.64 ( 2.4H, m), 4.60 – 4.53 ( 0.4H, m), 4.36-4.14 ( 1.2H, m), 3.77-3.62 ( 1 H, m).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,1254073-41-0, 5-Fluoropicolinohydrazide, and friends who are interested can also refer to it.

Reference:
Patent; GLAXO GROUP LIMITED; DEAN, David Kenneth; MUNOZ-MURIEDAS, Jorge; SIME, Mairi; STEADMAN, Jon Graham Anthony; THEWLIS, Rachel Elizabeth Anne; TRANI, Giancarlo; WALTER, Daryl Simon; WO2010/125102; (2010); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

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. 1254073-41-0, name is 5-Fluoropicolinohydrazide, the common compound, a new synthetic route is introduced below. Recommanded Product: 1254073-41-0

The title compound was prepared in an analogous method to that described in E1 11. To a solution of 4-[(2-chlorophenyl)carbonyl]-2-piperazinone (I4) (225 mg, 0.943 mmol) in Dichloromethane (5 ml) stirred under argon at room temp was added solid triethyloxonium tetrafluoroborate (179 mg, 0.943 mmol). The reaction mixture was stirred at RT for 2 hr. Solid 5-fluoro-2-pyridinecarbohydrazide (I24) (161 mg, 1.037 mmol) was added and the reaction mixture stirred at RT for 18 hr. The solvent was evaporated in vacuo, and the residue dissolved in n-butanol (5 ml) and stirred at 120 0C for 4 hr. The reaction mixture was cooled to room temperature and partitioned between Dichloromethane (~ 25 ml) and saturated brine (~ 25 ml). The aqueous phase was extracted wih Dichloromethane (2 x 25 ml) and the combined organic extracts washed with saturated brine (~ 25 ml), dried over sodium sulphate, and evaporated in vacuo to afford the crude product as a yellow oil. This was dissolved in 1 :1 MeOH:DMSO and purified by Open Access Mass Directed AutoPrep on Sunfire C18 column using Acetonitrile Water with a Formic acid modifier. The solvent was evaporated in vacuo and the residue dried overnight in a vacuum oven at 40 0C to give the required product as a white powder in 126.4 mg.LCMS: 2 minute run in MeCN. MH+ m/z = 358.03; RT = 0.80-0.82 min.

The synthetic route of 1254073-41-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLAXO GROUP LIMITED; DEAN, David Kenneth; MUNOZ-MURIEDAS, Jorge; SIME, Mairi; STEADMAN, Jon Graham Anthony; THEWLIS, Rachel Elizabeth Anne; TRANI, Giancarlo; WALTER, Daryl Simon; WO2010/125102; (2010); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem