Synthetic Route of 5932-30-9, A common heterocyclic compound, 5932-30-9, name is Ethyl 5-phenyl-1H-pyrazole-3-carboxylate, molecular formula is C12H12N2O2, 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.
To a solution of compound 23 (l.08g, 5.00 mmol) and compound 25 (981 mg, 6.00 mmol) in 50 ml acetonitrile was added K2CO3 (1.24 g, 9.00 mmol) and heated to reflux for 8 hours. After cooled to rt, filtered off, the filtrate was concentrated and the residue was purified by silica-gel column chromatography to afford compound 24a (950 mg, 55% yield) and compound 24b (150 mg, 8.7% yield).(compound 24a)LCMS m/z=344 [M+H]+ LC/MS informationColumn: Xbridge C18 (3.5pm 4.6x50mm)Flow rate: 1.8 mL/min UV detection wavelength: 254nmMobile phase’- [A] is 0.05% TFA-containing aqueoous solution, and [B] is 0.05% TFA- containing acetonitrile solutionFrom 0 to 1.5 minutes, the percentage of [B] in the mobile phase was gradually increased from 5% to 100%. Thereafter a solution of 100% of [B] was used as the mobile phase.retention time= 1.41 minutes.(compound 24b)LCMS m/z=344 [M+H]+ LC/MS informationColumn: Xbridge C18 (3.5mu?iota 4.6x50mm)Flow rate: 1.8 mL/minUV detection wavelength: 254nmMobile phase: [A] is 0.05% TFA-containing aqueoous solution, and [B] is 0.05% TFA- containing acetonitrile solutionFrom 0 to 1.5 minutes, the percentage of [B] in the mobile phase was gradually increased from 5% to 100%.. Thereafter a solution of 100% of [B] was used as the mobile phase.retention time= 1.50 minutes
The synthetic route of 5932-30-9 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Shionogi & Co., Ltd.; YUKIMASA, Akira; WO2012/144661; (2012); A1;,
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