Source of materialTo asolutionof3,4,5-trimethoxybenzoic acid (1.06g,5.0 mmol) in anhydrousdichloromethane and acatalytic amount of DMF, oxalyl chloride (1.27 g, 10.0mmol) was added at room temperature. The reaction was stirred at room temperature for 3hand then evaporated under reduced pressure. The residue was triturated with dichloromethane and evaporated. The acid chloride was then dissolved in dichloromethane and added dropwise to asolution of 4-(4-methoxyphenyl)-6-phenylpyridin-2-amine (1.16 g, 4.2 mmol) ,triethylamine (1.2 ml, 8.4 mmol) and catalytic amounts of DMAP in dichloromethane at 273-278K. The reaction was monitored by TLC(thin layer chromatography), and the product wasisolated afterwashing thereactionmixture with asaturated aqueous NaCl solution, dried over anhydrous Na 2 SO 4 ,and evaporated. The residue was further purified by columnchromatography (PE/EA =8 :1) to give the title compound as ac olourless solid, m.p.: 453-454K. Yield 1.43 g, 72% [1].Finally, 10 mg of the title compound were dissolved in am ixture of PE/EA( 1:3, v/v), and the solution was kept at room temperature for five days. Naturale vaporation gave whiten eedle-shaped crystals suitable for X-ray diffraction analysis.
DiscussionRecently, much attention has been paid to pyridine and its derivatives due to their wide applications in different fields of medicine and material chemistry, most of which have potential biological activity [2,3 ]. There are two crystallographically independant moleculesinthe asymmetric unit of the title crystal structure, in which all bond lengths are within normal ranges. There are three benzene rings and one pyridine ring in each molecule. In both molecules, the pyridine ring is nearly coplanar with the benzene ring containing atomsC 1t oC 6, and C29 to C34, respectively. The torsion angles of C18-N2-C17-N1, C46-N4-C45-N3, C17-N2-C18-C19 and C45-N4-C46-C47 are 170.
