GERMANIUM. XII. TETRA-ALKYL AND TETRA-ARYL COMPOUNDS OF GERMANIUM. GERMANIUM TETRA-ETHOXYL¹

Abstract

July, 1925GGRMANIUM ARYL AND ALKYL COMPOUNDS 2039 6 or more moles of sodium hydroxylamine disulfonate which rapidly hydrolyzed to an acid solution of monosulfonate.Preparation of Dimethylg1yoxime.-The biacetyl monoxime and monosulfonate were filtered to remove any sediment, mixed in a 15-liter flask, the mixture was heated to 70" and allowed to remain warm and occasionally stirred for several hours. The dimethylglyoxime separated in crystals that were filtered from the solution after it had become cold. They were washed with cold water until free from sulfate; yield, 575 g. ; 235-240'.Recrystallization was unnecessary since the product was pure white and free from tarry matter. SummaryA study has been made of the conditions affecting the formation of dimethylglyoxime, and simplified and efficient methods have been devised for the preparation of biacetyl monoxime, sodium hydroxylamine monosulfonate and dimethylglyoxime.

Synthesis and Spectroscopic Characterisation of Some Neutral Tetracoordinated Germanium (IV) Alkoxyalkanolates

“…13 Germanium 2 and isopropanol 9 were estimated as reported earlier. All manipulations were performed in a moisture free environment.…”

“…1 H NMR spectra: The 1 H spectra of all these redistilled complexes exhibit characteristic peaks. 13 C NMR spectra: In the 13 C NMR spectra, the position and the number of alkoxyalkanol carbon signals are as expected ( Table 3). No appreciable shift was observed in the position of alkoxyalkanol protons which were observed at their expected positions, ruling out the possibility of coordination through the oxygen atom of alkoxyalkanol moiety 12 (Table 2).…”

Synthesis and Characterization of Some New Metallo-Organic Derivatives of Germanium(IV)

“…All manipulations were performed in a moist free environment. Ge(OR)4 {where R = Et, Pr i } were prepared according to the literature method 15 . Germanium 16 , ethanol and isopropanol 17 were estimated as reported earlier.…”

Synthesis and Characterisation of Modified Germanium (IV) Isopropoxide with Internally Functionalised oximes: Soft Transformation of Some of These to Pure Nano-Sized Germania

“…Hazardous benzene was handled with all the necessary precautions. Germanium tetraisopropoxide 27 and oximes 28 were synthesised and purified according to the literature methods. Germanium 29 4 (1.70 g; 5.5 m mol) was added to a benzene solution (~15 ml) of [HONC(Me)C 5 H 4 N-2] (1.50 g; 11.0 m mol).…”