Preparation and properties of ".BETA.1 and .BETA.2"-isomers of the salicylato(triethylenetetramine)cobalt(III) complex.

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概要

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• β-Salicylato(triethylenetetramine)cobalt(III) chloride monohydrate has been obtained from salicylic acid and β-dichloro(triethylenetetramine)cobalt(III) chloride at pH 10–11. The separation of "β<SUB>1</SUB> and β<SUB>2</SUB>" isomers was attempted by using ion exchange. The IR spectra of the "β<SUB>1</SUB> and β<SUB>2</SUB>" complexes showed four strong absorption peaks in the 990–1100 cm<SUP>−1</SUP> region. This indicates that the complexes assume the β-form. The <SUP>1</SUP>H-NMR spectrum of ammine protons of coordinated triethylenetetramine of the β<SUB>1</SUB> complex showed six signals with an intensity ratio of 1:1:1:1:1:1, while that of the β<SUB>2</SUB> complex showed five signals with an intensity ratio of 1:1:1:1:2, in 1.8 mol dm<SUP>−3</SUP> D<SUB>2</SUB>SO<SUB>4</SUB>. The order of the chemical shifts in ppm is N(2)H<N(3)H<N(4)H<SUB>2</SUB><N(1)H<SUB>2</SUB>. Thus, the protons of the secondary N(3)H of coordinated triethylenetetramine absorb at lower fields than the terminal N(1)H<SUB>2</SUB> protons. The <SUP>13</SUP>C-NMR spectra of the "β<SUB>1</SUB> and β<SUB>2</SUB>" complexes in heavy water showed six signals for trienligand carbons and seven signals for salicylato-ligand carbons. The spectra of these complexes have shown two different configurations of the "β<SUB>1</SUB> and β<SUB>2</SUB>" complexes.

• 公益社団法人 日本化学会の論文

著者

• Yamamoto Yoshihisa

  Faculty Of Engineering Kyushu University

• Toyota Eiko

  Faculty of Pharmaceutical Science, Higashi Nippon Gakuen University

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