摘要
A series of gallium derivatives incorporating with pincer type tridentate symmetric and asymmetric pyrrolyl ligands are conveniently synthesized. Compilation of a symmetrical tridentate pyrrole ligand, [C 4 H 2 NH-(2,5-CH 2 NH t Bu) 2 ] (1) with one equiv of n-BuLi in heptane generates lithiated 1 that turns to Ga[C 4 H 2 N-(2,5-CH 2 NH t Bu) 2 ]Cl 2 (2) subjecting the addition of GaCl 3 /ether suspension into diethyl ether. Reacting 2 with two equiv of lithium reagents (LiR) in same solvent originates a series of gallium compounds Ga[C 4 H 2 N-(2,5-CH 2 NH t Bu) 2 ]R 2 (3, R = Me; 4, R = O-C 6 H 4 -4-Me; 5, R = O-C 6 H 3 -2,6-Me 2 ) in moderate yield through metathesis reactions. Furthermore, the combination of a tridentate asymmetrical pyrrole ligand, [C 4 H 2 NH(2-CH 2 NH t Bu)(5-CH 2 NMe 2 )] and n-BuLi initiates the lithiated 6 that undergoes the formation of a penta-coordinated gallium compound GaCl 2 [C 4 H 2 N(2-CH 2 NH t Bu)(5-CH 2 NMe 2 )] (7) while reacting with GaCl 3 . Furthermore, reacting 7 with two equivs of MeLi affords the gallium-alkyl compound, GaMe 2 [C 4 H 2 N(2-CH 2 NH t Bu)(5-CH 2 NMe 2 )] (8) in high yield. The Ga-derivatives are characterized by 1 H and 13 C NMR spectroscopy and the molecular structures of 2, 3, 4, 5 and 7 are determined by single crystal X-ray diffractometry in solid state. © 2013 Elsevier B.V. All rights reserved.