TY - JOUR
T1 - Synthesis and protonolysis of neutral aluminum dihydride compounds stabilized by tridentate-substituted pyrrolyl ligands
T2 - Synthesis, structural characterization and ring-opening polymerization of ε-caprolactone
AU - Chang, Jr Chiuan
AU - Chen, Ya Chi
AU - Datta, Amitabha
AU - Lin, Chia Her
AU - Hsiao, Ching Sheng
AU - Huang, Jui Hsien
N1 - Funding Information:
We thank the National Science Council of Taiwan for the financial support, the National Computing Center for High Performance for databank searching, and the National Changhua University of Education for the X-ray structure analyses.
PY - 2011/11/15
Y1 - 2011/11/15
N2 - A series of aluminum compounds containing tridentate pyrrolyl ligands were obtained from related aluminum dihydride compounds via protonolysis. Treatment of tetranuclear aluminum compound [C4H2N{2,5-(CH 2NMe2)2}Al2H5] 2 (1) with two equivalents of [C4H3N{2,5- (CH2NMe2)2}] in methylene chloride at 0 °C led to the formation of [C4H2N{2,5-(CH2NMe 2)2}]AlH2 (2). Similarly, when the deuterated aluminum compound 1D was used, the corresponding aluminum compound [C 4H2N{2,5-(CH2NMe2) 2}]AlD2 (2D) could be isolated. The reaction of 2 with one or two equivalents of phenylethyne, triphenylmethanethiol, 2,6- diisopropylaniline, or triphenylsilanol generated mononuclear aluminum compounds [[C4H2N{2,5-(CH2NMe2) 2}]AlRR′ (3, R = -CCPh, R′ = H; 4, R = R′ = -CCPh; 5, R = -SCPh3, R′ = H; 6, R = R′ = -SCPh3; 7, R = -NH(2,6-iPr2Ph), R′ = H; 8, R = R′ = -NH(2,6-iPr2Ph); 9, R = -OSiPh3, R′ = H; 10, R = R′ = -OSiPh3). Related Al-D compounds of 3, 5, 7 and 9 were also synthesized and corresponding IR spectroscopic data well matched in comparison of the stretching frequencies of Al-H and Al-D. The molecular structures of 2D, 4, 5, 5D, 7, and 10 have been determined by X-ray crystallography. Compounds 2, 5, and 7 initiated the ring-opening polymerization of ε-caprolactone and produced high-molecular weight of poly-ε-caprolactone.
AB - A series of aluminum compounds containing tridentate pyrrolyl ligands were obtained from related aluminum dihydride compounds via protonolysis. Treatment of tetranuclear aluminum compound [C4H2N{2,5-(CH 2NMe2)2}Al2H5] 2 (1) with two equivalents of [C4H3N{2,5- (CH2NMe2)2}] in methylene chloride at 0 °C led to the formation of [C4H2N{2,5-(CH2NMe 2)2}]AlH2 (2). Similarly, when the deuterated aluminum compound 1D was used, the corresponding aluminum compound [C 4H2N{2,5-(CH2NMe2) 2}]AlD2 (2D) could be isolated. The reaction of 2 with one or two equivalents of phenylethyne, triphenylmethanethiol, 2,6- diisopropylaniline, or triphenylsilanol generated mononuclear aluminum compounds [[C4H2N{2,5-(CH2NMe2) 2}]AlRR′ (3, R = -CCPh, R′ = H; 4, R = R′ = -CCPh; 5, R = -SCPh3, R′ = H; 6, R = R′ = -SCPh3; 7, R = -NH(2,6-iPr2Ph), R′ = H; 8, R = R′ = -NH(2,6-iPr2Ph); 9, R = -OSiPh3, R′ = H; 10, R = R′ = -OSiPh3). Related Al-D compounds of 3, 5, 7 and 9 were also synthesized and corresponding IR spectroscopic data well matched in comparison of the stretching frequencies of Al-H and Al-D. The molecular structures of 2D, 4, 5, 5D, 7, and 10 have been determined by X-ray crystallography. Compounds 2, 5, and 7 initiated the ring-opening polymerization of ε-caprolactone and produced high-molecular weight of poly-ε-caprolactone.
KW - Aluminum
KW - Pyrrole
KW - Ring-opening polymerization
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U2 - 10.1016/j.jorganchem.2011.08.021
DO - 10.1016/j.jorganchem.2011.08.021
M3 - Article
AN - SCOPUS:80053904916
SN - 0022-328X
VL - 696
SP - 3673
EP - 3680
JO - Journal of Organometallic Chemistry
JF - Journal of Organometallic Chemistry
IS - 23
ER -