Twofold Borylation of Benzene Derivatives with (Diisoalkylamino)boradiyl UnitsThe reaction of subvalent boron species generated by the defluorination of difluoro(diorganylamino)borane with Na/K alloy in the presence of 1,4‐disubstituted benzene derivatives leads to products which contain two (diorganylamino)boradiyl units and two remaining double bonds which are located on the substituted C atoms. Compounds 5 to 8 exhibit structures based on a 2,8‐diborabicyclo[3,2,1]octa‐3,6‐diene skeleton while 9 shows a skeleton with a 1,3a,4,6a‐tetrahydroborolo[3,2‐b]borole structure. The latter structure corresponds to that of 1 obtained in the same reaction with benzene. The compounds are characterized by elemental analyses and spectroscopically [MS, NMR (1H, 11B, 13C, 15N, 19F, 29Si)]. X‐ray structure analyses are presented for 1, 6, 7, 8, and 9.
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