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Original Articles

Improved Synthesis of 1,2-Dichlorotetramesityldigermane and Other Mesitylgermanes

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Pages 1205-1217 | Received 08 Nov 1995, Accepted 11 Apr 1996, Published online: 21 Aug 2006

References

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  • It is important to determine accurately the concentration of the Grignard reagent in each reaction. The amount of Grignard reagent/GeCl4 is adjusted each time to give exactly a 2:1 ratio of MesMgBr:GeCl4
  • The composition of the reaction mixture from the Mes2GeHLi/Mes2GeCl2 coupling reaction can vary depending on the quality of the tert-BuLi used to generate the germyllithium reagent. If the mixture consists of Mes4Ge2HCl/Mes2GeH2/Mes4Ge2H2, the quantity of reagents for chlorination is adjusted based on the Mes4Ge2HCl/Mes2GeH2/Mes4Ge2H2 ratio as determined by 1H NMR spectroscopy. If the mixture consists of Mes4Ge2HCl/Mes2GeCl2, flash chromatography through a 6 silica gel column can be performed at this stage to give pure Mes4Ge2HCl before chlorination

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