Source of materialAcetic acid (0.4 g) was added to a solution of ethyl 3-amino-2-N-[(2¢-cyanobiphenyl-4-yl)methyl]aminobenzoate (2.0 g) in ethyl orthocarbonate (10 mL). The mixture was stirred at 353 K for one hour. The reaction mixture was concentrated, and the concentrate was dissolved in ethyl acetate. The solution was washed with an aqueous solution of sodium hydrogen carbonate and water. The solvent was evaporated to give crystals. Colorless single crystals of title compound suitable for diffraction analysis were obtained from an ethyl acetate solution after one week.
Experimental detailsThe disordered ethyl group was split into two positions and the atomic positions were refined under using of restraints for CO and CC bond lengths. While the C atoms of the major part could be refined anisotropically, the respective atoms of the minor part had to be refined isotropically.
Discussion
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