These common heterocyclic compound, 51985-95-6, name is Methyl 5-hydroxy-1-methyl-1H-pyrazole-3-carboxylate, 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. Product Details of 51985-95-6
Methyl 5 -hydroxy- i-methyl- 1H-pyrazole-3 -carboxylate (I Med. Chem., 54:8174 (2011)) (0.35 g, 2.24 mmol), K2C03 (0.62 g, 4.48 mmol), and sodium chlorodifluoroacetate (0.684 g, 4.48 mmol) were dissolved in DMF (10 mL) and water (1 mL). The reaction was heated to 130 °C for 20 mm. The reaction was diluted with water (100 mL) and EtOAc (200 mL). The organic phase was separated, washed with water(5x) and brine, dried (Na2SO4) and concentrated. The residue was purified by flash chromatography (0-80percent EtOAc/Hex gradient) to give Intermediate 14A (0.3 73 g, 81percent yield) as a colorless syrup. MS(ESI) m/z: 207.0 (M+H) ?H NMR: (400 MHz, CDC13) oe ppm 6.44 (t, J=i.0 Hz, 1H), 6.46 (t, J=72.2 Hz, 1H), 3.92 (s, 3H), 3.82 (s, 3H); ?9F-NMR:(376 MHz, CDC13) oe ppm -84.02 (s, 2F).
The synthetic route of Methyl 5-hydroxy-1-methyl-1H-pyrazole-3-carboxylate has been constantly updated, and we look forward to future research findings.
Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; LADZIATA, Vladimir; GLUNZ, Peter W.; HU, Zilun; WANG, Yufeng; (0 pag.)WO2016/10950; (2016); A1;,
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