The products of the reduction of dihalogeno(diorganylamino)boranes with LiAIHj in toluene depend upon the steric requirement of the aminosubstituents.' It shows that upon using different procedures to produce sec.amino(dihydro)boranes the results depend critically from the solvent, the stoichiometry of the educts and the temperature applied beyond the sterical factors. However, certain procedures are preferably used to produce distinct moieties. Eight procedures (in part using different ratios of the educts) were applied and evaluated for their results. Mixtures of products were explored by NMR and MS. Pure compounds are characterized by NMR: Η, Β, C, MS and elemental analyses or high resolution MS. An X-ray structure analysis is presented for 26b.
The 1,4-dithia-2,6-diaza-3,5-diborinanes 1a-d react with elemental sodium with formation of the 1,3-diaza-2,4-diboretidines 2a-d. By use of more sodium in case of 1 d or 3,5-bis(diethylamino)- 2-cyclohexyl-6-trimethylsilyldiborinane, the 1,3-thiaza-2,4-diboretidines 3 were formed. 3.5-Dimethyl-2,6-bis(trimethylsilyl)-1,4-dithia-2,6-diaza-3,5-diborinane gives the borazine 4, The reaction of di-t-butyl-sulfurdiimide with 2,6-di-t-butyl-3,5-dimethyl-1,4-dithia-2,6-diaza-3,5-diborinane leads by ring contraction to the four-membered ring system 5. 1H, 11B, 13C NMR and mass spectra are reported and discussed.
Abstract The reaction of trimethylsilylsulfonamides with halodiorganylboranes leads to the corresponding sulfonamidoboranes and halotrimethylsilane. Trimethylsilylsulfonamides are prepared by reaction of the corresponding sulfonyl chlorides with primary amines, followed by the addition of chlorotrimethylsilane in the presence of excess triethylamine. 1H, 11B NMR spectra and mass spectra are reported
Dichlorocarbene generated in aprotic systems reacts with bis[(2,6-dimethylphenyl)trimethylsilylamino]germanium(ll) to give 2,3-dichloro-8-methyl-2-[(2,6-dimethy lphenyl)trimethylsily lamino]-1-trimethylsilyl-1-aza-2-germa-1,2,3,4-tetrahydronaphthalene, 1, or chloro-bis[(2,6-dimethylphenyl)trimethylsilylamino]-trichloromethylgermanium(IV), 2, depending upon the preparation of the dichlorocarbene. From 1,3-bis(trimethylsilyl)-1,3-diaza-2-germa(ll)indane and dichlorocarbene, 2-[(tert.-butoxy)chloromethyi]-2-chloro-1,3-bis(trimethylsilyl)-1,3-diaza-2-germaindane, 3, and 2-bis(tert.butoxy)methyl-2-chloro-1,3-bis(trimethylsilyl)-1,3-diaza-2-germaindane, 4, were obtained. The compounds are characterized by 1 H-and 13 C-NMR and mass spectrometry, 1 and 3 also by elemental analyses. X-ray structure analyses were performed for 1 and 2.
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