[Optical spectral verification of a harmful impurity to palladium catalyst].
The condensation of glyoxal with benzylamine leaded to hexabenzyl-hexaazaisowurtzitane (HBIW) with formic acid catalyst, and at the same time some side products were produced. Some impurities in HBIW would be harmful to the palladium catalyst used in the hydrogenolysis of HBIW, subsequently resulting in the low yield or failure of the catalytic reaction. The impurities in hexabenzylhexaazaisowurtzitane were distilled by means of recrystal technic, which were isolated by preparative chromatograph. The structure of the main impurity was studied with FTIR, 1H-NMR, ESI-MS, and element analysis. The result shows that the structure is comfirmed as N,N'-dibenzyl-oxalamide. which was synthesized in the way reported in the literature, and was charactered by FTIR, 1H-NMR and EI-MS. And the optical spectra data of the sample synthesized and the substance isolated from the impuries were the same, testifying that the substance isolated was N, N'-dibenzyl-oxalamide ulteriorly. N, N'-dibenzyl-oxalamide was added in the hydrogenolysis system of HBIW catalyzed by Pd catalyst. The result shows that N, N'-dibenzyl-oxalamide can reduce the activity of Pd catalyst, and when the quantity of N,N'-dibenzyl oxalmine added achievs 0.9% of the weight of HBIW, the reaction of catalytic hydrogenolysis fails.
Chen
Hua-xiong
HX
School of Material Science and Engineering, Beijing Institute of Technology, Beijing 100081, China. nanfei314@126.com
Chen
Shu-Sen
SS
Hu
Feng-xia
FX
Li
Li-jie
LJ
Yang
Rong-jie
RJ