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ChemicalBook CAS DataBase List 5-PYRIDIN-3-YL-1H-PYRAZOLE-3-CARBOXYLIC ACID

5-PYRIDIN-3-YL-1H-PYRAZOLE-3-CARBOXYLIC ACID synthesis

3synthesis methods
-

Yield:374064-01-4 90%

Reaction Conditions:

with sodium hydroxide in tetrahydrofuran;methanol;water at 65; for 4 h;

Steps:



A mixture of NaOH (0.06 g, 15 mmol), PPCAE (1.763 g, 8 mmol), THF (16 ml), MeOH (15 ml) and H2O (8 ml) was stirred at 65 °C for 4 h. After removal of the solvent under reduced pressure. The residue obtained was diluted with water, a cold aqueous HCl solution (6 mol/L) was used to neutralize the solution to pH 5. The white precipitate was collected and washed with water to give crude HPPC (1.361 g, 90%). The crude HPPC was purified on silica gel by column chromatography. HPPC (Fig. A.2): IR (KBr, γ, cm-1): 3423(s), 1724(s), 1573(w), 1438(w), 1389(w), 1337(m), 1292(m), 1243(m), 762(s), 703(s), 636(w). MS(ESI): m/z (%) = 233.8 [HPPC+HCOOH]-, 223.9[HPPC+Cl]-, 188.1 [HPPC+H]-.

References:

Zhao, Hong;Chu, Zhao-Jing;Gao, Gui-Yuan;Huang, Huan-Huan;Qu, Zhi-Rong [Polyhedron,2014,vol. 83,p. 143 - 149]

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