211. The chromatography of gases and vapours. Part IX. The preparation of some mixed hexa-alkyldigermanes and the elucidation of their isomer ratios

Abstract

A number of mixed hexa-alkyldigermanes have been prepared from germanium tetrachloride by using mixed organometallic reagents. The isomer ratios of several of these compounds have been determined by gas-liquid-chromatographic methods.TETRA-ALKYL and tetra-aryl derivatives of monogermane are most frequently prepared by the reaction of germanium tetrachloride with a Grignard reagent2 Rijkens and Glockling and Hooton4 have discussed how the normal course of this reaction can be affected by reductive coupling and by steric hindrance. Phenyl-,4 ~i n y l -, ~ and ethyl-magnesium bromide react with germanium tetrachloride to give, respectively, 69% (but only in the presence of an excess of magnesium), 25%, and 8% yields of the corresponding digermanes,

Gas Chromatography

“…This includes studies of the catalytic redistribution reactions of alkyl groups associated with the elements Si, Ge, and Pb (500) , the separation and determination of linear and cyclic polydimethylsiloxanes (668), the elucidation of isomer ratios in the preparation of some mixed hexa-alkyldigermanes (558), and the separation of organotin compounds (300, 496,616) and alkylchlorosilanes (530). A flame ionization detector gave 20% greater response to silicon compounds than to analogous carbon compounds (499).…”