逆相ペーパークロマトグラフィーによるブチルスズ化合物の分離,確認
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概要
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The separation and the identification of some butyl-tin compounds (Bu<SUB><I>n</I></SUB>SnX<SUB>4<I>n</I></SUB>) are achieved by the reversed phase paper chromatography. Liquid paraffin is best fitted for the stationary phase among several drainage substances tested, including kerocene, decaline and a low-polymer of trifluorochloroethylene.<BR>The ascending method is adopted on development. Developers used are water-miscible solvents added with water and acid or base, <I>e. g</I>. acetone-water-acetic acid (100:50:5), butanol saturated with 2<I>N</I> HCl, or acetone-water-lutidine (100:50:50).<BR>The acids are necessary to prevent the tailing of spots in the chromatogram, but the addition of base hinders the traveling of spots on the paper.<BR>The butyl-tin compounds are detected by the spraying of dithizone in tetrachloromethane or of diphenylcarbazone in methanol, but Bu<SUB>4</SUB>Sn should be preliminarily oxidized by the ultraviolet ray irradiation before the spraying.<BR>The compounds gave the following R<SUB>f</SUB>-values on the acetone-water-acetic acid (100:50:5) system, <BR>Bu<SUB>4</SUB>Sn … 0.00 Bu<SUB>3</SUB>SnCl … 0.50<BR>Bu<SUB>2</SUB>SnCl<SUB>2</SUB> … 0.82 BuSnCl<SUB>3</SUB> … severe tailing and on the <I>n</I>-propanol-water-acetic acid (100:100:5) system, <BR>Octyl<SUB>2</SUB>SnC1<SUB>2</SUB> … 0.69 Bu<SUB>2</SUB>SnCl<SUB>2</SUB> … 0.95.<BR>BuSnCl<SUB>3</SUB> and stannic chloride did not give a well-defined chromatogram on the paper treated with liquid paraffin, but showed a good result on the un-treated paper in <I>n</I>-butanol saturated with 2<I>N</I> HCl, giving the following R<SUB>f</SUB> values:<BR>BuSnCl<SUB>3</SUB> ……… 0.86 SnCl<SUB>4</SUB> …… 0.67<BR>Bu<SUB>2</SUB>SnCl<SUB>2</SUB> ……… 1.00<BR>The developments of the products of Grignardreagent with stannic chloride and the disproportionation between Bu<SUB>4</SUB>Sn and stannic chloride gave good separation and identification of these compounds (Fig. 6 and 7).