Abstract
A pentacoordinate 1,2-oxagermetanide 1, K + 18-crown-6 [−C 6H 4C(CF 3) 2O−]GePh[−CH(CH 2 tBu)C(CF 3) 2O−] −, was quantitatively synthesized as a colourless block (m.p. 217–218°C (decomp.)) by deprotonation of the corresponding ß-hydroxygermane 2, [−C 6H 4C(CF 3) 2O−]GePhCH(CH 2 tBu)C(CF 3) 2OH, which can be prepared by unique cycloelimination of benzene from o-HO(CF 3) 2CC 6H 4GePh 2[CH(CH 2 tBu)C(CF 3) 2OH] ( 3). On heating in CD 3CN at 150°C for 30 days, 1 equilibrates with another diastereomer 4 and then undergoes the Peterson-type reaction to give the corresponding olefin 5, (F 3C) 2C=CHCH 2 tBu (13%), and its double-bond migrated isomer 6, (F 3C) 2CHCH=CH tBu (33%). The yields of the olefins 5 and 6 are not very high, because their polymerization takes place under the reaction conditions. X-ray crystallographic analysis of 1 shows that it has a distorted trigonal bipyramidal structure with two oxygen atoms at apical positions.
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