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1Author    Lothar Weber, Eckhard Dobbert, Andreas Rausch, Hans-Georg Stammler, Beate NeumannRequires cookie*
 Title    Synthesis, Structure and Reactivity of 2-Amino-and 2-Imino-2,3-dihydro-1H -1,3,2-diazaboroles  
 Abstract    The 2-halo-2,3-dihydro-1H-1,3,2-diazaboroles RN-CH=CH-N(R)BX (la': R = rBu, X = Br; lb: R = 2,6-Me2C6H.v, X = I) were converted into the 2-amino-2,3-dihydro-\H -1,3,2-diazaboroles RN-CH=CH-N(R)B-NH2 (2a: R = /Bu; 2b: 2,6-Me2C6H3) by treatment with dry gaseous ammonia. Similarly reaction of la' with 2,6-dimethylaniline or /BuNHt afforded the corresponding derivates /BuN-CH=CH-N(rBu)BNHR' (3; R 1 = 2,6-Me2C6H3; 4; R1 = rBu). The treatment of la' with the ethylene diamine adduct of lithium acetylide led to the formation of [rBuN-CH=CH-N(/Bu)BN(H)CH2]2 (5). Lithiation of 2 a and subsequent silylation gave 6 (R1 = SiMe3), which was transformed to the diborolylamine [/BuN-CH=CH-N(rBu)B]2NH (7) upon exposure to la'. Borolylketimine /BuN-CH=CH-N(/Bu)B-N=CPh2 (8) and borolylcar-bodiimide fBuN-CH=CHN(/Bu)B-N=C=N-SiMe3 (9) resulted from la' and Ph2C=NSiMe3 or Me3SiN=C=NSiMe3, respectively. All the new compounds were characterized by elemental analyses as well as spectroscopic data (IR, 'H, n B, i3C NMR, MS). Heterocycle 5 was also subjected to an X-ray diffraction analysis. 
  Reference    Z. Naturforsch. 54b, 363—371 (1999); eingegangen am 25. September 1998 
  Published    1999 
  Keywords    Boron, Diazaboroles, Amines, Imines 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-0363.pdf 
 Identifier    ZNB-1999-54b-0363 
 Volume    54 
2Author    S. HuRequires cookie*
 Title    One-Pot Preparation of o-Xylylene Diam ine and its Related Am ines  
 Abstract    -ich i K a w a h a ra a n d T ad afu m i U c h im a ru * D epartm ent A m ethod for one-pot preparation of o-xyly-lene diamine, 1,8-diaminomethylnaphthalene, and l,2,4,5-tetrakis(aminomethyl)benzene has been developed. The procedure is simpler and the yield of the reaction is higher than by the conven­ tional method. 
  Reference    Z. Naturforsch. 55b, 985—987 (2000); received May 18 2000 
  Published    2000 
  Keywords    Amines, Halides, Staudinger Reaction 
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 TEI-XML for    default:Reihe_B/55/ZNB-2000-55b-0985_n.pdf 
 Identifier    ZNB-2000-55b-0985_n 
 Volume    55 
3Author    G. S., M. K.Requires cookie*
 Title    Preparation of Spin-Labeled Phosphoroamidates in High Yield Using Imidazole as the Transfer Agent  
 Abstract    The spin-labeled (l-oxyl-2,2,6,6-tetramethyl-4-piperidyl)-phenyl imidazole-1-phos-phonate (4) was used to prepare (l-oxyl-2,2,6,6-tetramethyl-4-piperidyl)phenyl N-alkyl and N-aryl phosphoroamidates (8) in yields generally exceeding 70%. @ > -0 -P -N R 'R " ^ -0 -P -C I OR OR OR 4 8 1 0 Amidates 8 were also prepared from the corresponding chloridate 10. However, in the 
  Reference    (Z. Naturforsch. 32b, 321—327 [1977]; received September 3 1976) 
  Published    1977 
  Keywords    Spin-Labeled Phosphoroamidates, Amines, N itroxyl Moiety, Transphosphorylation 
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 TEI-XML for    default:Reihe_B/32/ZNB-1977-32b-0321.pdf 
 Identifier    ZNB-1977-32b-0321 
 Volume    32 
4Author    Ulrich Knips, Friedo HuberRequires cookie*
 Title    Umsetzungen von Monomethylthalliumdiacetat mit Aminen Reactions of Monomethylthallium Diacetate and Amines  
 Abstract    Decomposition of MeTl(OAc)2 (Me = CH3, HO Ac = CH3COOH) in methanol in the presence of amines, like 2-, 3-and 4-picoline, benzylamines, dimethylaniline causes mainly N-methylation; the concurring O-methylation of acetate, giving MeOAc, is only of minor importance. The rate of N-methylation increases in the series 2-picoline < pyridine < 3-picoline < 4-picoline < dimethylaniline < dime thy lbenzylamine. Picolinic acid and MeTl(OAc)2 (molar ratio 1:1) react to give 25% N-methylpicolinic acid and 75% MeOAc; when the molar ratio was at least 2:1, a 1:1 mixture of N-methylpicolinic acid and the methylester of picolinic acid was produced. These results and rate changes in different solvents are explained by assuming MeT10Ac+ being the active methylthallium electro-phile. Der geschwindigkeitsbestimmende Schritt beim Zerfall von Monomethylthalliumverbindungen MeTlX2 (Me = CH3, X = z.B. CH3COO) in Lösung kann als S^-Angriff des jeweils stärksten Nukleo-phils oder konkurrierender Nukleophile (Anion und Solvensmoleküle) im Reaktionssystem an der Tl-gebundenen Methylgruppe von MeTlX+ verstanden werden, das im Dissoziationsgleichgewicht mit MeTlX2 vorliegt [1,2]. Weitere Untersuchungen der Zerfallsreaktion in Gegenwart organischer Amine, über die wir nachfolgend berichten, bekräftigen diese Vorstellung und erlauben Aussagen über den Einfluß von Nukleophilie und Basizität der Reak-tanden bei diesen Zersetzungsreaktionen. Ergebnisse Beim Zerfall von MeTl(OAc)2 in methanolischer Lösung in Gegenwart von 2-, 3-und 4-Picolin ent-standen in allen Fällen als Hauptprodukte die ent-sprechendenN-Methylpicoliniumacetate und T10 Ac. Daneben bildete sich Essigsäuremethylester (MeOAc) in einer von der verwendeten Base ab-hängigen Menge: So wurden bei Verfolgung des Zerfalls von MeTl(OAc)2 in Gegenwart von 2-bzw. 3-bzw. 4-Picolin nach 20 h bei einer Reaktions-temperatur von 30 °C etwa 15 bzw. 5 bzw. 2-3% MeOAc (bezogen auf die berechnete maximale Menge von MeOAc als einziges Zerfallsprodukt) gefunden. 
  Reference    Z. Naturforsch. 38b, 434—436 (1983); eingegangen am 20. Dezember 1982 
  Published    1983 
  Keywords    Monomethylthallium Diacetate, Amines, Methylation, Reaction Rate 
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 TEI-XML for    default:Reihe_B/38/ZNB-1983-38b-0434.pdf 
 Identifier    ZNB-1983-38b-0434 
 Volume    38 
5Author    RostislavD. Lampeka, Zam Ira, D. Uzakbergenova, VictorV. SkopenkoRequires cookie*
 Title    Spectroscopic and X-Ray Investigation of Cobalt(III) Complexes with 2-Oximinocarboxylic Acids  
 Abstract    Mixed complexes of Co(III) with 2-oximinopropionic (H 2A) or 2-oximino-3-phenylpropionic (H 2B) acid and different amine (imidazole, benzimidazole, pyridine, yS-picoline, y-picoline) are reported. Characterization of the complexes was based upon ele­ mental analysis, conductivity and JR, 'H N M R, and electronic absorption spectra, and X-ray diffraction analysis. The organic ligands behave as 0 ,N donors via the carboxyl oxygen and the oxime nitrogen atoms. A trans-octahedral structure has been assigned to the bis(2-oximino-carboxylato)bis(am ine)cobalt(III) on the basis of 'H N M R data. The crystal and molecular structures of the complexes rra«5-[bis(2-oximinopropionato)bis-(imidazole)]-(I) and ^ • a«5'-[bis(2-oximinopropionato)bis(pyridine)]cobalt(III) (II) were deter­ mined. I crystallizes in space group P 2/« with a = 14.167(2), b = 8.774(_1), c = 14.785(2)Ä, ß = 113.37(1)°, Z = 4, Dca)c = 1.568 g e m '3. II crystallizes in space group P 1 with a = 9.122(2), b = 10.038(2), c = 11.759(2) A, a = 69.95(1)°, ß = 67.47(2)°, y = 69.49(2)°, Z = 2, Dcalc = 1.547 g-cm~3. The structures were refined to unweighted R factors of 0.036 and 0.028, respec­ tively. The coordination sphere around Co is pseudo-octahedral with the 2-oxim inopropionato ligands occupying four equatorial positions, and the amines in axial po­ sitions. 
  Reference    Z. Naturforsch. 48b, 409—417 (1993); received November 2 1992 
  Published    1993 
  Keywords    Cobalt, Oximiocarboxylic Acid, Amine, X-Ray 
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 TEI-XML for    default:Reihe_B/48/ZNB-1993-48b-0409.pdf 
 Identifier    ZNB-1993-48b-0409 
 Volume    48 
6Author    BerndW. Rackmeyer1 ', Saqib Alib, Wolfgang Storch0, Martina VosteencRequires cookie*
 Title    2-[N,N-Bis(trimethylstannyl)amino]pyridine and Bis[N-(N-trimethyIsiIyI- 2-aminopyridyI)]dimethyltin -Intramolecular N-Sn Co-ordination  
 Abstract    2-[N,N-Bis(trimethylstannyl)amino]pyridine (1), bis[N-(N-trimethylsilyl-2-aminopyridyl)]-dimethyltin (2) and bis[N-(N-trimethylsilyl-2-amino-3-methyl-pyridyl)]dimethyltin (3) were prepared and characterized by 'H, i3C, l5N, 29Si and ll9Sn NMR spectroscopy. In the case of 1, intramolecular pyridine-N-Sn co-ordination was established by the low temperature ll9Sn NMR spectra which show two resonance signals, one for a penta-co-ordinate and one for a tetra-co-ordinate tin site. In the cases of 2 and 3, intramolecular pyridine-N-Sn co-ordination follows conclusively from l3C, l5N and ll9Sn NMR parameters. In contrast with the known behaviour of the corresponding trimethyltin derivative, the methyl group in 3-position of the pyridine ring does not prevent this type of co-ordination in 3. 
  Reference    Z. Naturforsch. 54b, 1165—1169 (1999); received June 17 1999 
  Published    1999 
  Keywords    Tin, Amines, Pyridine, Co-ordination, NMR Data 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-1165.pdf 
 Identifier    ZNB-1999-54b-1165 
 Volume    54 
7Author    Bernd Wrackmeyer3, Jürgen Weidinger3, Heinrich Nöthb, Wolfgang Storchb, Thomas Seifertb, Martina VosteenbRequires cookie*
 Title    Determination of Coupling Signs 17 (119Sn, 15N ) and 2/ ( 119Sn, 117Sn) in Trimethylstannylamines  
 Abstract    The l5N-labelled trimethylstannylamines 1 -3 [(M e3Sn)3N, (M e3Sn)2NPh, (M e3Sn)2N-BCgHi4 (BCgHi4 = 9-borabicyclo[3.3.0]nonyn and the non-labelled 4, Me3 Sn-N(BC8Hi4)2 , were prepared and studied by 1H, 1 C, l5N and l9Sn NMR. The l5N ultrahigh resolution NMR spectra of 1 revealed otherwise unobserved parameters such as 2/ (15N ,S n ,'C) and the isotope induced chemical shift 2 zAl2/l3C (l5N). ll9Sn NM R spectra of 1, recorded under similar con­ ditions, also show new parameters such as V (' |ySn,N,Sn,l3C) which are not resolved in the non-labelled derivative. By using various types o f two-dimensional heteronuclear shift corre­ lations, absolute coupling signs o f l7 (l l9 Sn,15N) (all < 0) in 1 -3 were determined. By the same techniques it proved possible to confirm the negative sign o f :7(Sn,Sn) (-195.4 Hz) in 1. In contrast, the coupling constants 27(Sn,Sn) for 2 (+71.7) and 3 (+62.0) possess a positive sign. This sign inversion, observed here for the first time for apparently similar compounds, demonstrates the enormous influence o f substituents on the nature o f the lone pair o f electrons at the nitrogen atom. It also shows that these experiments for sign determinations o f coupling constants are necessary in order to interpret these data correctly. 
  Reference    Z. Naturforsch. 53b, 1494—1500 (1998); received July 30 1998 
  Published    1998 
  Keywords    Tin, Amines, NM R Data, Ultrahigh Resolution, Coupling Sign Determination 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-1494.pdf 
 Identifier    ZNB-1998-53b-1494 
 Volume    53 
8Author    G. S.Requires cookie*
 Title    Reactions of tert-Butylperoxy Esters, XIII Reactions of Dialkyl ie/t-Butylperoxy Phosphates with A m inesa,b,c  
 Abstract    The interaction of dialkyl tert-butylperoxy phosphates, (R 0)2P (0)0 0 C M e3 (1) with primary and secondary cycloalkylamines, R 'R " N H , R' = cyclo-CeH^, R " = H ; R '= R " = cyclo-C6H n (2) in the presence and absence of water, produces the corre­ sponding dialkyl cycloalkyl ammonium phosphates, (R 0)2P (0) 0 -N +H 2R " R / (3), and ierJ-butanol. In carbon tetrachloride the reaction produces in addition to 3 the corre­ sponding cyclohexylammonium chloride, discussed. 
  Reference    (Z. Naturforsch. 30b, 724—731 [1975]; received February 17 1975) 
  Published    1975 
  Keywords    fer£-Butylperoxy Esters, Dialkyl Cycloalkylammonium Phosphates, feri-Butylperoxy Phosphates, Dialkyl Phosphates, Amines 
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 TEI-XML for    default:Reihe_B/30/ZNB-1975-30b-0724.pdf 
 Identifier    ZNB-1975-30b-0724 
 Volume    30