Carl Habben

Struktur und bindungsverhältnisse von 1,4-dithia-2,6-diaza-3,5-diborinanen

Abstract 1,3-Disubstituted sulfur diimides react with 3,5-dialkyl- and 3,5-diaryl-1,2,4-tri-thia-3,5-diborolanes, respectively, to give 1,4-dithia-2,6-diaza-3,5-diborinanes. The 1 H, 11 B, 13 C, 14 N, 29 Si NMR and mass spectra and the results of X-ray analyses of crystalline 2-t-butyl-6-(1,3-dimethyl-1,3,2-diazaborolidinyl)-3,5-dimethyl- and 2-t-butyl-6-(2,6-dimethylphenyl)-3,5-diphenyl-1,4-dithia-2,6-diaza-3,5- are reported and correlated.

Reaktionen vonN-Sulfinylverbindungen mit dem 1,2,4-Trithia-3,5-diborolan-Ringsystem und Substitutionsreaktionen am 1,2,4-Trithia-3,5-diborolan und 1,2-Dithia-4-aza-3,5-diborolidin

The reaction of trimethylsilyl- and pentafluorophenyl-N-sulfinylamine respectively with 3,5-dihalogeno-1,2,4-trithia-3,5-diborolanes yields the 1,2-dithia-4-aza-3,5-diborolidines1-3.Tert-butyl-N-sulfinylamine and 3,5-dimethyl-1,2,4-trithia-3,5-diborolane react analogous. OtherN-sulfinylamines however split the disulfane bridge in 3,5-dimethyl-1,2,4-trithia-3,5-diborolane and the 1,4-dithia-2-aza-3,5-diborolidines5A-7(A) are formed. Besides of boroxines, cyclo-2,4,6-trimethyl-1,3-dioxa-5-aza-2,4,6-triboranes and cyclo-2,4,6-trimethyl-1-oxa-3,5-diaza-2,4,6-triboranes are formed as byproducts,8–10 have been isolated. In 1,2,4-trithia-3,5-diborolanes and 1,2-dithia-4-aza-3,5-diborolidines the bromo-atoms can be substituted by alkyl (13, 14), by amino (15–20) and by isothiocyanato groups. The compounds were characterised analytically and spectroscopically (MS; NMR:1H,11B,19F,29Si; IR).

Synthesis and X-Ray crystal structure of a tricyclic lead-nitrogen-boron heterocycle

1,3,5,7-Tetra-t-butyl-4,8-Biphenyl-1,3,5,7-tetra-aza-2,6-diplumba-4,8-diboratricyclo[4.2.0.02,5]octane-1,5-diium-2,6-diide(1)hasbeen obtained from PhB(NButLi)2 and PbCl4in hexane or from PbCl2 intetrahydrofuran and structurally characterised by X-ray diffraction.

Synthese und Charakterisierung von 1,3-dithia-2-boryl-[3]ferrocenophanen

Abstract The 1,3-dithia-2-boryl[3]ferrocenophanes (I-VIII) are obtained from the reaction of ferrocene-1,1′-dithiol ( A ) with dihalogenorganylboranes by elimination of the hydrogenhalides. I-VIII can be also prepared by starting from Fe(C 5 H 4 SLi) 2 · 2THF ( B ) inplace of A , but in lower yields. The air-sensitive [3] ferrocenophanes have been characterized analytically and spectroscopically (MS; NMR: 1 H, 11 B, 13 C).

Synthese und Eigenschaften von 2,3-Dihydro-4H-1,3,2-thiazaborin-4-onen

3-Bromo-1,2,3-dithiaboroles react with Grignard reagents by formation of 3-al-kyl(aryl)-1,2,3-dithiaboroles, which, upon reaction with isocyanates leads to the 2,3-dihydro-4H-1,3,2-thiazaborine-4-ones. 1H, 11B, 13C NMR and mass spectra are described and discussed.

Synthese und Kristallstruktur von 2,4-Di-tert-butyl-3-pentafluorphenyl-1,2,4,3-thiadiazaboretidin / Synthesis and Crystal Structure of 2,4-Di-tert-butyl-3-pentafluorophenyl-1,2,4,3-thiadiazaboretidine

Sulfur-diimides react with bismethylmercapto-pentafluorophenylboranes by reductive 1,3-cycloaddition of the NSN-sequence and formation of the 1,2,4,3-thiadiazaboretidines 2a,b. NMR (1H, 11B, 13C, 19F, 29Si), mass spectra and the results of the X-ray structure analysis of 2 a are reported and discussed.

Notizen: Molekül- und Kristallstruktur des 2,4-Bis(diisopropylamino)-3-phenyl-1,3,2,4-thiazadiboretidins / Crystal and Molecular Structure of 2,4-Bis(diisopropylamino)-3-phenyl-1,3,2,4-thiazadiboretidine

The title compound, C18H33B2N3S, isolated from the reaction of 3,5-bis(diisopropylamino)-1,2,4,3,5-dithiazadiborolidine with elemental sodium, crystallizes in space group P1̅ with cell constants a = 1034.3(6), b = 1230.4(8), c = 1728.5(12) pm, α = 97.50(6), β = 97.95(5), γ = 90.17(5)° and Z = 4. X-ray structure refinement converged at R = 0.087, wR = 0.085, w-1 = σ2(F0) + 0.004 Fo2. The fourmcmbered ring B2NS is planar, the angle B—S—B being 70°.

Synthese und Kristallstruktur von l,3-Di-tert-butyl-4,4-di-methyl-2-pentafluorphenyl-4,2-stannabora-cyclobutan / Synthesis and Crystal Structure of 1,3-Di-tert-butyl-4,4-di-methyl-2-pentafluorophenyl-4,2-stannabora-cyclobutane

The synthesis and crystal structure of 1,3-di-tert-butyl-4,4-dimethyl-2-pentafluorophenyl-1,3,4,2-diazastannoboracyclobutane are reported.

Synthese und Eigenschaften von 1,2,7,3,6-Thiadiazadiborepinen, Kristallstruktur des 2,7-Di-tert-butyl-3,6-dimethyl-3,6-dihydrobenzo-1,2,7,3,6-thiadiazadiborepins / Syntheses and Properties of 1,2,7,3,6-Thiadiazadiborepines, Crystal Structure of 2,7-Di-tert-butyl-3,6-dimethyl-3,6-dihydrobenzo-1,2,7,3,6-thiadiazadiborepin

2,5-Bisdimethylamino-2,5-dihydrobenzo[b]-1,2,5-thiadiborole (2) has been obtained from the diiodine-derivative by reaction with dimethyl-aminotrimethylsilane. Reaction of 2 or 2,5-bisdimethylamino-1′,2′-dimethyl-2,5-dihydrobenzo[b]-thiadiborole with di-tert-butyl-, tertbutyl-trimethylsilyl- and bistrimethylsilyl-sulfurdiimide yields the 2,7,3,6-tetrahydrobenzo[b]-1,2,7,3,6-thiadiazadiborepines (3a-3e). 1H, 11B, 13C NMR, MS and analytical data and results of analysis are given. For 3a the X-ray structure is reported.

1,4-Dithia-2,6-diaza-3,5-diborinane: Ein neues B–N–S-Ringsystem/ 1.4-Dithia-2.6-diaza-3,5-diborinanes: A Novel B – N –S-Ringsystem

Abstract The novel 1,4-dithia-2,6-diaza-3,5-diborinane ring system results from the reaction of 3,5- dialkyl- (or di-sec.amino-) substituted 1,2,4-trithia-3,5-diborolanes with 1.3-disubstituted sulfurdiimides by replacement of the disulfane bridge. Upon treatment with azomethines, 3,5-dibromo- 1.2.4-trithia-3,5-diborolane gives 3,5-dibromo-1,2-dithia-4-aza-5-diborolidines by substitution of the sulfur atom in position 4. 1H , 11B , 13C, 29Si NMR and mass spectra are reported and discussed.