Abstract
A series of aluminum alkoxide and bis-alkoxides compounds were synthesized and characterized. Reacting 1 with 1 and 2 equiv. of t-butanol in methylene chloride generates [C4H3N(CH2NMe2)-2]2Al(O-t-Bu) (2) and [C4H3N(CH2NMe2)-2-H-C4H3N(CH2NMe2)-2]Al(O-t-Bu)2 (3) in 47% and 54% yield, respectively. The 1H NMR spectrum of 2 exhibits two singlets for NMe2 and CH2N at δ 2.52 and 3.84, respectively, representing the symmetrical manner of molecular structure 2 in a solution. Compound 3 is not thermal stable in solution which decompose into substituted pyrrole ligand C4H4N(CH2NMe2)-2 and unknown aluminum alkoxides. Reacting 1 with 2 equiv. of triphenylsilanol in methylene chloride generates a tetra-coordinated aluminum "ate" compound [C4H3N(CH2NMe2)-2-H- C4H3N(CH2NMe2)-2]Al(OSiPh3)2 (4) in 49% yield. The 1H NMR spectra of 4 at room temperature show a broad signal at δ 1.57 for NMe2 fragments and the signals for CH2N were not observed. VT 1H NMR spectra of 4 show the NMe2 fragments became two singlets (δ 1.27 and 2.12) and the CH2N exhibited two doublets (δ 2.44 and 3.56) at 240 K. The fluxional energy barrier (ΔG‡) is estimated at ca. 50 kJ/mol. The molecular structures of compounds 3 and 4 are determined by single-crystal X-ray diffractometer.
| Original language | English |
|---|---|
| Pages (from-to) | 3718-3722 |
| Number of pages | 5 |
| Journal | Journal of Organometallic Chemistry |
| Volume | 692 |
| Issue number | 17 |
| DOIs | |
| Publication status | Published - 2007 Aug 1 |
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All Science Journal Classification (ASJC) codes
- Biochemistry
- Physical and Theoretical Chemistry
- Organic Chemistry
- Inorganic Chemistry
- Materials Chemistry
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Synthesis of aluminum alkoxide and bis-alkoxide compounds containing bidentate pyrrolyl ligands. / Lin, Che Yu; Lee, Hon Man; Huang, Jui-Hsien.
In: Journal of Organometallic Chemistry, Vol. 692, No. 17, 01.08.2007, p. 3718-3722.Research output: Contribution to journal › Article
TY - JOUR
T1 - Synthesis of aluminum alkoxide and bis-alkoxide compounds containing bidentate pyrrolyl ligands
AU - Lin, Che Yu
AU - Lee, Hon Man
AU - Huang, Jui-Hsien
PY - 2007/8/1
Y1 - 2007/8/1
N2 - A series of aluminum alkoxide and bis-alkoxides compounds were synthesized and characterized. Reacting 1 with 1 and 2 equiv. of t-butanol in methylene chloride generates [C4H3N(CH2NMe2)-2]2Al(O-t-Bu) (2) and [C4H3N(CH2NMe2)-2-H-C4H3N(CH2NMe2)-2]Al(O-t-Bu)2 (3) in 47% and 54% yield, respectively. The 1H NMR spectrum of 2 exhibits two singlets for NMe2 and CH2N at δ 2.52 and 3.84, respectively, representing the symmetrical manner of molecular structure 2 in a solution. Compound 3 is not thermal stable in solution which decompose into substituted pyrrole ligand C4H4N(CH2NMe2)-2 and unknown aluminum alkoxides. Reacting 1 with 2 equiv. of triphenylsilanol in methylene chloride generates a tetra-coordinated aluminum "ate" compound [C4H3N(CH2NMe2)-2-H- C4H3N(CH2NMe2)-2]Al(OSiPh3)2 (4) in 49% yield. The 1H NMR spectra of 4 at room temperature show a broad signal at δ 1.57 for NMe2 fragments and the signals for CH2N were not observed. VT 1H NMR spectra of 4 show the NMe2 fragments became two singlets (δ 1.27 and 2.12) and the CH2N exhibited two doublets (δ 2.44 and 3.56) at 240 K. The fluxional energy barrier (ΔG‡) is estimated at ca. 50 kJ/mol. The molecular structures of compounds 3 and 4 are determined by single-crystal X-ray diffractometer.
AB - A series of aluminum alkoxide and bis-alkoxides compounds were synthesized and characterized. Reacting 1 with 1 and 2 equiv. of t-butanol in methylene chloride generates [C4H3N(CH2NMe2)-2]2Al(O-t-Bu) (2) and [C4H3N(CH2NMe2)-2-H-C4H3N(CH2NMe2)-2]Al(O-t-Bu)2 (3) in 47% and 54% yield, respectively. The 1H NMR spectrum of 2 exhibits two singlets for NMe2 and CH2N at δ 2.52 and 3.84, respectively, representing the symmetrical manner of molecular structure 2 in a solution. Compound 3 is not thermal stable in solution which decompose into substituted pyrrole ligand C4H4N(CH2NMe2)-2 and unknown aluminum alkoxides. Reacting 1 with 2 equiv. of triphenylsilanol in methylene chloride generates a tetra-coordinated aluminum "ate" compound [C4H3N(CH2NMe2)-2-H- C4H3N(CH2NMe2)-2]Al(OSiPh3)2 (4) in 49% yield. The 1H NMR spectra of 4 at room temperature show a broad signal at δ 1.57 for NMe2 fragments and the signals for CH2N were not observed. VT 1H NMR spectra of 4 show the NMe2 fragments became two singlets (δ 1.27 and 2.12) and the CH2N exhibited two doublets (δ 2.44 and 3.56) at 240 K. The fluxional energy barrier (ΔG‡) is estimated at ca. 50 kJ/mol. The molecular structures of compounds 3 and 4 are determined by single-crystal X-ray diffractometer.
UR - http://www.scopus.com/inward/record.url?scp=34447277627&partnerID=8YFLogxK
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U2 - 10.1016/j.jorganchem.2007.05.013
DO - 10.1016/j.jorganchem.2007.05.013
M3 - Article
AN - SCOPUS:34447277627
VL - 692
SP - 3718
EP - 3722
JO - Journal of Organometallic Chemistry
JF - Journal of Organometallic Chemistry
SN - 0022-328X
IS - 17
ER -