Reference of 15802-75-2, A common heterocyclic compound, 15802-75-2, name is 4-Iodo-3-methyl-1H-pyrazole, molecular formula is C4H5IN2, 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.
Under nitrogen protection,To a 10 ml Schlek reaction tube (a glass instrument commonly used in anaerobic operation)Bromo-5- (4- (6-bromopyridyl-3) phenyl) pyridine, 2.2 mmol of 3-methyl-4-iodopyrazole-0.02 mmol palladium acetate,0.05 mmol dicyclohexyl (3,6-dimethoxy-2 ‘, 4′, 6′-triisopropyl (1,1′-biphenyl) -2-yl)5.0 mmol of potassium t-butoxide, and 5 ml of dioxane, the reaction tube was purged with nitrogen three times,And then heated to 110 C with an oil bath under magnetic stirring, and the reaction was refluxed for 24 hours. Down to room temperatureThe reaction solution was further added, 5.0 mmol of 3,5-dicarboxyphenylboronic acid, 0.03 mmol of palladium acetate, 0.06 mmol2′-dicyclohexyl-2,6-dimethoxy-3-sulfonic acid-1,1’-biphenyl sodium salt, 10.0 mmol potassium carbonate,And 200 mmol of water; then heated to 100 C with an oil bath under magnetic stirring,The reaction was refluxed for 40 hours. Down to room temperature; add 20 ml of water, filtration, with concentrated hydrochloric acid to adjust the pH of the filtrate to 1,After stirring at room temperature for 6 h, the mixture was filtered, washed with ethanol and dried to give product 22 in 68% yield.The mass spectrum (ESI) of the product (C40H28N6O8) was 720.20.
The synthetic route of 15802-75-2 has been constantly updated, and we look forward to future research findings.