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Modification of aluminium alkoxides with dialkylmalonates.

Lichtenberger R, Baumann SO, Bendova M, Puchberger M, Schubert U - Monatsh. Chem. (2010)

Bottom Line: Al(malonate)3 (malonate = dimethyl, diethyl, di-iso-propyl and di-tert-butyl malonate), Al2(OiPr)4(malonate)2 (malonate = di-iso-propyl and di-tert-butyl malonate), Al2(OiPr)2(di-iso-propylmalonate)4 and Al3(OH)(OEt)3(diethylmalonate)5.An Al2(OiPr)2(dialkylmalonate)4 derivative was only obtained by disproportionation of Al2(OiPr)4(di-iso-propylmalonate)2, but not by reaction of Al(OiPr)3 with dialkylmalonates in the corresponding molar ratio.Reactions of Al(OtBu)3 only resulted in Al(malonate)3 derivatives, but no transesterification was observed, contrary to the reaction of Al(OiPr)3 with dimethyl or diethyl malonate.

View Article: PubMed Central - PubMed

Affiliation: Institute of Materials Chemistry, Vienna University of Technology, Vienna, Austria.

ABSTRACT

Abstract: Depending on the reaction conditions, different aluminium dialkylmalonate derivatives were obtained by reaction of aluminium alkoxides Al(OR)3 (R = Et, iPr, tBu) with dialkylmalonates, viz. Al(malonate)3 (malonate = dimethyl, diethyl, di-iso-propyl and di-tert-butyl malonate), Al2(OiPr)4(malonate)2 (malonate = di-iso-propyl and di-tert-butyl malonate), Al2(OiPr)2(di-iso-propylmalonate)4 and Al3(OH)(OEt)3(diethylmalonate)5. All compounds were characterized by NMR spectroscopy, and single crystal structure analyses are reported for each type of compound. An Al2(OiPr)2(dialkylmalonate)4 derivative was only obtained by disproportionation of Al2(OiPr)4(di-iso-propylmalonate)2, but not by reaction of Al(OiPr)3 with dialkylmalonates in the corresponding molar ratio. Reactions of Al(OtBu)3 only resulted in Al(malonate)3 derivatives, but no transesterification was observed, contrary to the reaction of Al(OiPr)3 with dimethyl or diethyl malonate.

No MeSH data available.


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27Al NMR spectrum of 2d (in toluene-d8)
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Fig5: 27Al NMR spectrum of 2d (in toluene-d8)

Mentions: 27Al NMR spectra of 2c and 2d (Fig. 5) additionally supported the structure. Both spectra showed a broad signal assigned to tetrahedrally coordinated Al between 130 and 20 ppm with maxima at about 65 and 80 ppm, respectively, and one sharp signal at 5.1 or 4.8 ppm, assigned to octahedrally coordinated Al [7]. Integration of the signals revealed almost the expected 1:1 ratio, although integration is somewhat difficult because of the broad signal for tetrahedrally coordinated Al.Fig. 5


Modification of aluminium alkoxides with dialkylmalonates.

Lichtenberger R, Baumann SO, Bendova M, Puchberger M, Schubert U - Monatsh. Chem. (2010)

27Al NMR spectrum of 2d (in toluene-d8)
© Copyright Policy
Related In: Results  -  Collection

Show All Figures
getmorefigures.php?uid=PMC4494765&req=5

Fig5: 27Al NMR spectrum of 2d (in toluene-d8)
Mentions: 27Al NMR spectra of 2c and 2d (Fig. 5) additionally supported the structure. Both spectra showed a broad signal assigned to tetrahedrally coordinated Al between 130 and 20 ppm with maxima at about 65 and 80 ppm, respectively, and one sharp signal at 5.1 or 4.8 ppm, assigned to octahedrally coordinated Al [7]. Integration of the signals revealed almost the expected 1:1 ratio, although integration is somewhat difficult because of the broad signal for tetrahedrally coordinated Al.Fig. 5

Bottom Line: Al(malonate)3 (malonate = dimethyl, diethyl, di-iso-propyl and di-tert-butyl malonate), Al2(OiPr)4(malonate)2 (malonate = di-iso-propyl and di-tert-butyl malonate), Al2(OiPr)2(di-iso-propylmalonate)4 and Al3(OH)(OEt)3(diethylmalonate)5.An Al2(OiPr)2(dialkylmalonate)4 derivative was only obtained by disproportionation of Al2(OiPr)4(di-iso-propylmalonate)2, but not by reaction of Al(OiPr)3 with dialkylmalonates in the corresponding molar ratio.Reactions of Al(OtBu)3 only resulted in Al(malonate)3 derivatives, but no transesterification was observed, contrary to the reaction of Al(OiPr)3 with dimethyl or diethyl malonate.

View Article: PubMed Central - PubMed

Affiliation: Institute of Materials Chemistry, Vienna University of Technology, Vienna, Austria.

ABSTRACT

Abstract: Depending on the reaction conditions, different aluminium dialkylmalonate derivatives were obtained by reaction of aluminium alkoxides Al(OR)3 (R = Et, iPr, tBu) with dialkylmalonates, viz. Al(malonate)3 (malonate = dimethyl, diethyl, di-iso-propyl and di-tert-butyl malonate), Al2(OiPr)4(malonate)2 (malonate = di-iso-propyl and di-tert-butyl malonate), Al2(OiPr)2(di-iso-propylmalonate)4 and Al3(OH)(OEt)3(diethylmalonate)5. All compounds were characterized by NMR spectroscopy, and single crystal structure analyses are reported for each type of compound. An Al2(OiPr)2(dialkylmalonate)4 derivative was only obtained by disproportionation of Al2(OiPr)4(di-iso-propylmalonate)2, but not by reaction of Al(OiPr)3 with dialkylmalonates in the corresponding molar ratio. Reactions of Al(OtBu)3 only resulted in Al(malonate)3 derivatives, but no transesterification was observed, contrary to the reaction of Al(OiPr)3 with dimethyl or diethyl malonate.

No MeSH data available.


Related in: MedlinePlus