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. 5334-39-4, name is 3-Methyl-4-nitro-1H-pyrazole, A new synthetic method of this compound is introduced below., SDS of cas: 5334-39-4
A mixture of 3-methyl-4-nitro-lH-pyrazole (1.36 g, 10.71 mmol), tert-butyl-4- iodopiperidine-l-carboxylate (10.00 g, 32.14 mmol) and K2CO3 (2.96 g, 21.42 mmol) in DMF (16.6 mL) was stirred at reflux for 24 h. The reaction mixture was diluted with EtOAc and water and the layers were separated. The organic layer was washed with brine, dried over MgS04, filtered and was evaporated under reduced pressure. The residue was purified by column chromatography on silica gel (irregular SiOH 40 muiotaeta, 80 g, mobile phase: heptane/DCM, gradient from 50:50 to 0: 100). The pure fractions were combined and the solvent was evaporated to give a mixture of intermediate 349 and intermediate 349′ (540.00 mg, 16% yield). intermediate 350 intermediate 350′ At 0C, HC1 (4M in dioxane) (15.00 mL, 60.00 mmol) was added to a solution of a mixture of intermediates 349 and 349′ (0.54 g, 1.74 mmol) in 1,4-dioxane (4 mL). The reaction was stirred at rt overnight. The solvent was evaporated until dryness. The residue was taken up into DCM and basified with a 10% aqueous solution of K2C03. The organic layer was dried over MgS04, filtered and the solvent was evaporated until dryness. The residue (817 mg) was purified by column chromatography on silica gel (stationary phase: irregular SiOH, 15-40 muiotaeta, 40 g, mobile phase: 98% DCM, 2% MeOH (+ 10% NH4OH) to 95% DCM, 5% MeOH (+10% NH4OH)). The pure fractions were collected and the solvent was evaporated until dryness to give 0.480 g of a mixture of intermediates 350 and 350′ used as it for the next step.
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.