Synthetic Route of 52867-42-2, A common heterocyclic compound, 52867-42-2, name is Methyl 2-methyl-5-oxo-2,5-dihydro-1H-pyrazole-3-carboxylate, molecular formula is C6H8N2O3, 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.
Cyclopropanol (413 mg, 6.40 mmol) and methyl 5-hydroxy-2-methyl-pyrazole-3-carboxylate (1.0 g, 6.40 mmol) were suspended in anhydrous toluene (10.0 mL) prior to addition of triphenylphosphine (1.69 g, 6.40 mmol) and then di-tert-butylazodicarboxylate (1.47 g, 6.40 mmol). The reaction was heated to 110 C with stirring in a sealed vessel for 4.5 h, cooled & diluted with EtOAc (10 mL) and washed with water (10 mL). The organic layer was dried over Na2S04 and concentrated in vacuo. The crude product was purified by column chromatography eluting with a 0-100% gradient of EtOAc in isohexane. Product-containing fractions were combined and concentrated to afford the title compound (730 mg, 58% Yield). 6H (300 MHz, Chloroform-d) 6.31 (s, 1H), 4.04 (s, 3H), 3.91 (tt, J = 6.0, 3.0 Hz, 1H), 3.86 (s, 3H), 0.82 – 0.66 (m, 4H).
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.