Structural Diversity in Lithium Aryloxides, Part 1. Structurally Characterized [Li(OAr)(THF){sub x}]{sub n} where OAr = OC{sub 6}H{sub 5}, OC{sub 6}H{sub 4}(2-Me), OC{sub 6}H{sub 3}(2,6-Me){sub 2}, OC{sub 6}H{sub 4}(2-Pr{sup i}), OC{sub 6}H{sub 3}(2,6-Pr{sup i}){sub 2}, OC{sub 6}H{sub 4}(2-Bu{sup t}), OC{sub 6}H{sub 3}(2,6-Bu{sup t}){sub 2} Page: 6 of 120
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We have synthesized a series of Li(OAr) compounds in different solvents. Part 1 details
the "Li(OAr)(THF)x" adducts that were synthesized through the amide alcohol exchange reaction
shown in eq 3. The unhindered OPh was previously reported as [Li(OPh)(THF)]6 (THF =
tetrahydrofuran)8 and the sterically hindered DBP was found to adopt a dinuclear arrangement,
[Li(DBP)(THF)]215. Our investigation of sterically varied Li(OAr) in THF led to the isolation
of: [Li(OPh)(THF)]4 (1), [Li(oMP)(THF)]4 (2), [Li(DMP)(THF)]4 (3), [Li(oPP)(THF)]4 (4),
[Li(DIP)(THF)]3 (5), [Li(oBP)(THF)2]2 (6), and [Li(DBP)(THF)]2 (7). Solid and solution state
multi-nuclear NMR spectroscopy were used to determine the properties and structural aspects of
the THF adducts of Li(OAr) complexes. Part 223 of this study details the synthesis and
characterization of the structural diversity observed for the Li(OAr) isolated from pyridine
solutions as [Li(OAr)(py)x]2 (x = 2 for OAr = oMP, DMP, oPP, DIP, oBP; x = 1 for OAr =
DBP). Details of the syntheses and characterizations of these compounds are presented below.
Experimental
All compounds described below were handled with rigorous exclusion of air and water
using standard Schlenk line and glove box techniques. All solvents were freshly distilled from
the appropriate drying agent immediately prior to use.24The following chemicals were used as
received (Aldrich), stored, and handled under an argon atmosphere: H-OPh, H-oMP, H-DMP, H-
oPP, H-DIP, H-oBP, H-DBP, and LiN(SiMe3)2-
All solid state NMR spectra were obtained on an AMX-400 at 100.6, 155.5 and 58.9 MHz
for 3C, 'Li and 6Li, respectively. A 4 mm broadband MAS probe, spinning at 10 - 12.5 kHz, was
used for all experiments. For 3C, 12.5 kHz was used to reduce the overlap between the spinning
sidebands of the aromatic resonances with other peaks of interest. The 13C Cross Polarization
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Boyle,Timothy J.; Pedrotty, Dawn M.; Alam,Todd M.; Vick,Sara C. & Rodriguez, Mark A. Structural Diversity in Lithium Aryloxides, Part 1. Structurally Characterized [Li(OAr)(THF){sub x}]{sub n} where OAr = OC{sub 6}H{sub 5}, OC{sub 6}H{sub 4}(2-Me), OC{sub 6}H{sub 3}(2,6-Me){sub 2}, OC{sub 6}H{sub 4}(2-Pr{sup i}), OC{sub 6}H{sub 3}(2,6-Pr{sup i}){sub 2}, OC{sub 6}H{sub 4}(2-Bu{sup t}), OC{sub 6}H{sub 3}(2,6-Bu{sup t}){sub 2}, article, June 12, 2000; Albuquerque, New Mexico. (https://digital.library.unt.edu/ark:/67531/metadc711673/m1/6/: accessed April 24, 2024), University of North Texas Libraries, UNT Digital Library, https://digital.library.unt.edu; crediting UNT Libraries Government Documents Department.