GeR4 Compounds with R Cycloalkenyl

The pale yellow solid melts at 116°C with decomposition. Its NMR spectrum (In CDCI3) shows at 27°C a single broad resonance, 5 = 5.86 ppm, which broadens at lower temperature and below — 30°C splits into components which have been assigned to incompletely resolved AA BB X multiplets with 5(ppm) = 3.26 (H-1), 6.28 (H-3,4), and 6.63 (H-2,5) at —70°C (cf. Formula I). This behavior is consistent with rapid 1,2-metallotropic rearrangement above -30°C. 

For the preparation of this compound, the mixture of GeCl4 and C5H4CH3K (1 4 mole ratio) was reacted in CeHg for 48 h (74% yield). 

The compound has been isolated from the reaction of GeCl4 with 1-CgH7MgBr in ether. It melts at 196 to 198°C [1]. 

The compound is insoluble in ethanol and slightly soluble in ether or chloroform. It decomposes at 200°C [1]. 

---