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With sodium hydroxide; water; In ethanol; at 20℃; for 15h;
To a solution of pyridine-2-carboxamide (1.2 eq, 3.4 mmol, 0.41 g) in H2O (1.4 ml) and NaOH (1.5 eq, 4.3 mmol, 0.17 g), is added a solution of <strong>[6283-81-4]3-oxo-3-pyridin-3-yl-propionic acid ethyl ester</strong> (1eq, 2.85 mmol, 0.55 g) in EtOH (1.7 ml) at room temperature. The reaction is left to stir for 15 hours. The reaction solvent was removed under reduced pressure to give a solid residue. The crude product is purified by flash chromatography (DCM / MeOH 100:0 to 0:100) to afford 6-pyridin-3-yl-2-pyridin-2-yl-3H-pyrimidin-4-one as a white solid; MH+= 251
[Eu(pyridine-2-carboxamide)3(4,4'-dimethoxy-2,2'-bipyridine)].Cl3[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
A mixture of 10 mL methanolic solution of pyridine-2-carboxamide (0.3663 g, 3 mmol) and 10 mL methanolic solution of 4,4'-dimethoxy-2,2'-bipyridine (0.2162 g, 1 mmol) was stirred at room temperature for half an hour. Solution of EuCl3 was prepared by dissolving 1 mmol (0.2583 g) of EuCl3 in 10 mL of methanol and this solution was added to the ligands solution drop by drop with continuous stirring. The pH of resulting solution was maintained between 6 and 7. The reaction mixture was refluxed at 70 °C for 4 h. After refluxing for 4 h, the solution was cooled to room temperature and left as such overnight. Complex C1 was obtained as white precipitate which was filtered off, washed with methanol nd then dried under vacuum. The synthesis of complexes C2-C4 were done by adopting the same method as given above. Complex C2 was obtained from 3 mmol PCAO (0.3663 g), 1 mmol DMBP (0.2162 g) and1 mmol EuCl3 (0.2583 g), complex C3 was obtained from 3 mmol PDCA(0.4473 g), 1 mmol DMBP (0.2162 g) and 1 mmol EuCl3 (0.2583 g) and complex C4 was obtained from 3 mmol PM (0.3 mL), 1 mmol DMBP(0.2162 g) and 1 mmol EuCl3 (0.2583 g).
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