Accession Number:

ADA310565

Title:

Room Temperature Cyclopentadiene Elimination Reaction for the Synthesis of Diethylgallium-Amides, -Phosphides and -Thiolates, Crystal and Molecular Structures of Et2GaP(t-Bu)22 and Et2GaS(SiPh3)2.

Descriptive Note:

Technical rept.,

Corporate Author:

STATE UNIV OF NEW YORK AT BUFFALO DEPT OF CHEMISTRY

Report Date:

1996-06-24

Pagination or Media Count:

25.0

Abstract:

The compounds Et2GaNEt22, Et2GaNHMe2, Et2GaNHt-Bu2, Et2GaPi-Pr22, Et2GaPt-Bu22, and Et2GaSSiPh32 have been prepared in high yields at room temperature by the elimination of cyclopentadiene from Et2GaC5H5 and the corresponding amine, phosphine or thiol. The three diethylgallium amides and Et2GaPi-Pr22 are liquids whereas the other phosphide and the thiolate are crystalline solids at room temperature. All compounds were fully characterized by elemental analyses, 1H and 31P NMR spectroscopy and cryoscopic molecular weight studies in benzene, as appropriate and are dimeric in solution. The crystalline compounds Et2GaPt-Bu22 and Et2GaSSiPh32 were characterized by X-ray structural studies. Even though Et2GaNHt-Bu2 and Et2GaSSiPh32 were prepared at room temperature and isolated in high yield, 1H NMR studies revealed that neither compound was formed in high yield in solution. Removal of the cyclopentadiene by either dimerization or distillation, andor dimerization the gallium product are necessary to prevent the back reaction to reform the reactants.

Subject Categories:

  • Organic Chemistry
  • Inorganic Chemistry
  • Physical Chemistry
  • Crystallography
  • Atomic and Molecular Physics and Spectroscopy

Distribution Statement:

APPROVED FOR PUBLIC RELEASE