The origin of a common compound about 217073-76-2

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 217073-76-2, its application will become more common.

Some common heterocyclic compound, 217073-76-2, name is 1-(4-Fluorophenyl)-5-methyl-1H-pyrazole-4-carboxylic acid, molecular formula is C11H9FN2O2, 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. Recommanded Product: 217073-76-2

General procedure: To a solution of II (1-2 eq.) in dry DMF, dioxane or dichloromethane, particularly dry DMF (dimethylformamide) (3-10 ml) were added IV (1 mmol). HBTU (2-(lH-Benzotriazole-l-yl)- 1,1,3,3-Tetramethyluroniurn hexafluorophosphate) (1 -1.4 eq.), DIPEA (N,N- Diisopropylethylamine) (1-5 eq.) or triethylamine (5 eq.), particularly DIPEA, and optionally DMAP (4-Dimethylaminopyridine ) (0.1 eq.) were also added to the reaction mixture. The reaction temperature was usually in the range of from rt to 85 C, particularly rt. The reaction was usually allowed to process overnight (which as used herein specifies a duration of approximately between 12 and 24 h, depending on the reaction velocity). After completion of the reactions, the reaction solution was subjected to one or more after- treatments including: A) Extraction with organic solvents: The residue obtained from the reaction was dissolved in an organic solvent (such as ethyl acetate or dichloromethane) and was washed at least once with an aqueous 5% NaHC03, aqueous 5% citric acid and water. The organic layer was dried over magnesium sulfate and concentrated in vacuo. B) Chromatography: The crude product obtained from the reaction was purified by column chromatography on a silica gel flash column, by preparative TLC (thin layer chromatography) or preparative HPLC (high pressure liquid chromatography) with a defined eluent proportion. After completion of the reaction, the crude product was purified by siliga gel flash column chromatography (CHCl3/EtOH = 80:1 + 1 drop of HOAc). C) Recrystallization: The crude product was crystallized from ethanol (with activated carbon). D) Precipitation: After completion of the reaction, the reaction mixture was diluted with water, hexane or an aqueous Na2C03-solution and/or was poured into ice water and the formed precipitate was filtered off. E) Washing: The obtained solid (e.g. obtained by filtration) was washed with water, aqueous HC1 or Na2C03-solution and/or organic solvents. F) Suspending, followed by filtration: The crude product was suspended in Et20 (diethyether), filtered off and dried. G) Neutralization and recovery: After completion of the reaction, the solvent was evaporated in vacuo, water was added and the precipitate was formed. An aqueous 3% ammonia solution, or alternatively a sodium hydrogen carbonate solution was added to the suspension till pH = 8. After 30 min of stirring the precipitate was filtered off or the dissolved product was extracted

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 217073-76-2, its application will become more common.