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 35277-02-2 as follows. Safety of 4-Fluoro-1H-pyrazole
Add in 100mL round bottom flask1-bromo-N- (6-cyano-5-trifluoromethyl-pyridin-3-yl) -cyclobutanecarboxamide (0.30 g, 0.8618 mmol),4-fluoro-1H-pyrazole (0.148 g, 1.7236 mmol),Cuprous bromide dimethyl sulfide (17.7 mg, 0.08618 mmol),Triphenylphosphine (22.6 mg, 0.08618 mmol),Tripotassium phosphate (0.22 g, 1.0341 mmol),Sodium hydroxide (38 mg, 0.9480 mmol),10mL of anhydrous toluene was used as the solvent.The resulting mixture was heated to 50 C,Stir for 15 hours under argon protection.After confirming the completion of the reaction by thin layer chromatography,The reaction solution is cooled to 20 ¡À 5 ,Then add water (30 ml) and ethyl acetate (35 ml),After brief stirring, the liquid is separated,The organic phase was washed with brine (25 ml),Magnesium sulfate drying,filter,Drain the organic phase,An oily substance is obtained.Silica gel column chromatography separation (mobile phase is dichloromethane: ethyl acetate = 9: 1), purification,82 mg of yellow powder was obtained,Identified asN- (4-cyano-3-trifluoromethyl) phenyl-1- (4-fluoro-1H-pyrazol-1-yl) -cyclobutanecarboxamide.The yield is 27%.
According to the analysis of related databases, 35277-02-2, the application of this compound in the production field has become more and more popular.