GeR4 Compounds with R Substituted Alkyl

The compounds in this chapter are listed in Table 8. They have been prepared by the following methods. 

Reactions of RLi compounds with GeC resulted in only low product yield No. 8 was obtained from GeC and Si(CH3)3CH2Li in refluxing ether [43] GeCl4 and c-C6H- - CH2CH2Li in ether and subsequently in CeHe at 80 C for 2 h gave little of No. 12, c-C6Hii(CH2)4C6Hii-c, and considerable amounts of nondistillable resin. Details for a similar preparation of No. 14 were not reported [5]. A better yield of 

Method III Zn(CD3)2 and excess GeC were the starting materials in a small-scale preparation of No. 1 in a vacuum system (purification by vacuum distillation over KOH) [17]. Slow addition of Ge to Cd(CF3)2 CH3OCH2CH2OCH3 (1 2.4 mole ratio) in 1,4-dibromobutane and removal of volatile products as formed yielded No. 2 as the only CF3-containing germane [36, 38]. Alkylation of Ge with Hg(CF3)2 requires treatment at 150°C for 24 h to give a 20 to 40% yield of No. 1 [28, 31, 33]. A similar yield was obtained from GeBr4 and Hg(CF3)2 (1 2 mole ratio) in a sealed tube at 150°C Ge(CF3)3Br was the major product of this reaction and could to some extent be converted into No. 1 by further reaction with more Hg(CF3)2 [27, 28]. 

Further information on compounds preceded by an asterisk is given at the end of the table. Explanations, abbreviations, and units on p. XI. 

Ge(CD3)4 (Tables, No. 1). The fundamental modes of the vibrational spectra are given in Table 9. Some controversy in the assignment of the v(CH,CD) region of M(CH3)4 compounds (M = C to Pb) and their deuterated derivatives is discussed in [18] and includes the 

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