| | 1 | Author
| G. Alina, S. Z. Aitseva11 ', SergeyS K Arlova, ElenaS A Lekseyevaa, LeonidA A Slanova, EvgeniV A Vtom Onovb, JörgL. Orberthb | Requires cookie* | | | Title
| -Allylgermatrane. Synthesis, Structure and Reaction with Diazomethane  | | | | Abstract
| Reaction of allyltribromogermane (2), readily available from dibrom o(l,4-dioxane)ger-manium(II) (1) and allylbromide, with tris(2-tributylstannoxyethyl)-amine (4) gives 1-allylgermatrane (3) in almost quantitative yield. 3 crystallizes from /7-pentane as a colourless crystalline solid which was characterized by 'H and ,3C NMR spectroscopy and by an X-ray crystal structure study. The "atrane" skeleton shows a strong conformational disorder; the Ge-N distance of 2.208(3) A suggests the presence of a coordinative Ge-N bond. Treatment of 1 -allylgermatrane (3) with CH2N2 in the presence of catalytic amounts of Pd(OAc)2 affords 1-cyclopropylmethylgermatrane (5) in high yield. | | | |
Reference
| (Z. Naturforsch. 52b, 30—34 [1997]; received August 16 1996) | | | |
Published
| 1997 | | | |
Keywords
| Germanium, Germatrane, Cyclopropanation, X-Ray, NMR Spectra | | | |
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| default:Reihe_B/52/ZNB-1997-52b-0030.pdf | | | | Identifier
| ZNB-1997-52b-0030 | | | | Volume
| 52 | |
| 2 | Author
| Ralf Steudel, Monika Kustos, Andreas Prenzel | Requires cookie* | | | Title
| S | | | | Abstract
| y n t h e s is a n d S t r u c t u r e o f B i s [ d i(m e t h y lc y c lo p e n t a d ie n y l) c h lo r o -t it a n iu m ] t r is u lf id e [ (C p 2 C lT i)2S 3 ] -a R e a g e n t fo r T r is u lf id e L ig a n d T r a n s f e r R e a c t io n s [1] The dinuclear metallacycle of [Cp2Ti(/z-S2)2TiCp2] reacts with phosgene or thiophosgene to give [(CP2CITO2S3] which has been characterized by 1H and l3C NMR spectra as well as by an X-ray structure analysis. The trisulfido complex contains a helical TiSSSTi unit and may serve as an S3 transfer reagent in reactions with SCl-functional compounds. | | | |
Reference
| (Z. Naturforsch. 52b, 79—82 [1997]; received June 18 1996) | | | |
Published
| 1997 | | | |
Keywords
| Titanocene Complexes, Polysulfide Ligands, Structure, NMR Spectra | | | |
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| default:Reihe_B/52/ZNB-1997-52b-0079.pdf | | | | Identifier
| ZNB-1997-52b-0079 | | | | Volume
| 52 | |
| 4 | Author
| Lu | Requires cookie* | | | Title
| Synthesis of N,C,C-Trilithio-2,5-diaIlyl- pyrrole and its Solvent-Controlled Reactions with Electrophiles | | | | Abstract
| te d so lu tio n s ca n b e co o led to -80 °C w ith o u t p rec ip ita tio n . B e rn d W ra c k m e y e r5 5 B e rn d Schw arze Iris O rd u n g , 2,5-Diallylpyrrole 1 reacts with an excess of "BuLi in hexane/diethylether to give the N,C,C-trilithio reagent 2. 7Li NMR spectra of 2 in THF/ HMPTA at low tem perature indicate the pres ence of an ionic species. Reactions of 2 in TH F with electrophiles such as H 20 , D20 , Mel, Me3SiCl and Me3SnCl lead selectively to the cis-isomers 3a -6 a, whereas the analogous reactions in hexane or diethylether afford mixtures contain ing both cis-and rram-isomers (e.g. 3b). | | | |
Reference
| Z. Naturforsch. 52b, 427—430 (1997); received November 5 1996 | | | |
Published
| 1997 | | | |
Keywords
| Pyrrole, Solvent Controlled Reactions, NMR Spectra | | | |
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| default:Reihe_B/52/ZNB-1997-52b-0427_n.pdf | | | | Identifier
| ZNB-1997-52b-0427_n | | | | Volume
| 52 | |
| 5 | Author
| S. | Requires cookie* | | | Title
| Silaheterocyclen, XXXIII [1, 2]: Cycloadditions-Reaktionen des 1.1-Dichlor-2-neopentyIsilaethens mit Pentafulvenen | | | | Abstract
| ilaheterocycles, X X X III [1, 2]: C y c lo a d d itio n R e a c tio n s of 1 .1 -D ic h lo ro -2 -n eo p e n ty lsilen e w ith P e n ta fu lv e n e s N o rb e rt A u n er* , C la u s-R ü d ig e r H e ik e n w ä ld e r The reaction between in situ formed l,l-dichloro-2-neopentyl-l-silene, Cl2Si=CHCH2rBu (2), and 1,1-dimethylpentafulvene (5) leads to the formation of exo/endo-isomeric [4+2] cy-cloadducts 9 and [2+2] stereoisom ers 10 in good yields. NMR spectroscopic investigations of the product mixture prove the different modes of the silene cycloaddition reactions ([4+2] vs [2+2] addition). Treatment of 9 and 10 with LiA lH 4 and LiMe yield the stereo-and regioisomeric derivati ves (LiAlH 4: 16. 17; MeLi: 18, 19), whereas PhMgBr reacts with 10 to give only the mono substitution, the [4+2] com pound 20, and the diphenylated silacyclobutane 21. The reactions of silene 2 with pentafulvenes 6 -8 lead to similar results. | | | |
Reference
| Z. Naturforsch. 52b, 500—514 (1997); eingegangen am 19. Dezember 1996 | | | |
Published
| 1997 | | | |
Keywords
| Cycloaddition Reactions, Neopentylsilene, Pentafulvenes, NMR Spectra | | | |
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| default:Reihe_B/52/ZNB-1997-52b-0500.pdf | | | | Identifier
| ZNB-1997-52b-0500 | | | | Volume
| 52 | |
| 6 | Author
| Bernd Wrackmeyer, Jürgen Weidinger | Requires cookie* | | | Title
| N-Boryl-Substituted Bis(amino)stannylenes and -plumbylenes | | | | Abstract
| Two equivalents of N-lithio-N-trimethylsilyl-amino-9-borabicyclo[3.3.1]nonane (1) react with tin and lead dichloride by salt elimination to give the corresponding bis(amino)stannylene 2 and -plumbylene 3, respectively. The compounds 2 and 3 are monomers in solution and were characterized by 'H , i3C, 14N, 29Si, ll9Sn and 207Pb NMR spectroscopy. | | | |
Reference
| Z. Naturforsch. 52b, 947—950 (1997); received May 22 1997 | | | |
Published
| 1997 | | | |
Keywords
| Boron, Tin, Lead, Metal Amides, NMR Spectra | | | |
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| default:Reihe_B/52/ZNB-1997-52b-0947.pdf | | | | Identifier
| ZNB-1997-52b-0947 | | | | Volume
| 52 | |
| 7 | Author
| Max Herberhold, Volker Tröbs, Hong Zhou, Bernd Wrackmeyer | Requires cookie* | | | Title
| Reactivity and NMR Spectroscopic Properties of Tri(terf-butyl)plumbyl-amine | | | | Abstract
| Tri(rm-butyl)plumbyl-amine 1 was prepared and studied by one-(ID) and two-dimensional (2D) 'H, i3C, 5N and 207Pb NMR which allowed determination of the coupling signs /(Pb,13C) (> 0), 2y(207P b,'3C) (> 0), '7(207Pb,15N) (> 0; reduced coupling constant 1 A^(207Pb,I5N) < 0) and 27(207Pb-N-'H) (< 0). Transamination of 1 with aniline and pyrazole afforded the corresponding aniline (2) and pyrazole derivatives (3), respectively. N-Lithiation of 1, followed by treatment with Me3SiCl gave the tri(rm-butyl)plumbyl-trimethylsilyl-amine 5. The multinuclear magnetic resonance data of 2, 3 and 5 are presented. Trimethylplumbyl-phenyl-amine and trimethylplumbyl-ter/-butyl(dimethyl)silyl-amine were prepared and their NMR data were measured for comparison. | | | |
Reference
| Z. Naturforsch. 52b, 1181—1184 (1997); received July 14 1997 | | | |
Published
| 1997 | | | |
Keywords
| Lead, Organolead-nitrogen Compounds, NMR Spectra, Coupling Constants | | | |
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| default:Reihe_B/52/ZNB-1997-52b-1181.pdf | | | | Identifier
| ZNB-1997-52b-1181 | | | | Volume
| 52 | |
| 8 | Author
| Z. Naturforsch | Requires cookie* | | | Title
| Synthese und Reaktivität von 7-Triphenylstannyl-a-am inobuttersäure- derivaten | | | | Abstract
| Ph3SnCH2CH 2C H (NHCOOCH 2P h)COOCH3 (1) is synthesized by hydrostannation of methyl N-(benzyloxycarbonyl)vinylglycinate with Ph3SnH. The reaction o f 1 with HC1 in CH 3OH and with bromine in CHC13 yields the halostannylsubstituted compounds Ph3_"X,?SnCH2CH 2C H(NHCOOCH 2Ph)C OOCH3 (2 -4) (n = 1, 2; X = Cl, Br). By sapo nification with one equivalent of NaOH and subsequent acidification with HCl 1 is transformed into the free acid Ph3SnCH2C H 2C H(NHCOOCH2Ph)COOH (5) that undergoes cyclization into the 1,2-oxastanninane 6 with intramolecular elimination of benzene. IR, NMR data and the determination of the crystal structure of Ph2BrSnCH2CH2CH(NHCOOCH2Ph)COOCH3(3) reveal for 2 and 3 an intramolecular coordination of the N C (0)0-group at the tin atom to form a seven-membered ring. | | | |
Reference
| (Z. Naturforsch. 52b, 9—16 [1997]; eingegangen am 20. August 1996) | | | |
Published
| 1997 | | | |
Keywords
| Triphenylstannyl Aminobutyric Acid Derivatives, Halostannyl Aminobutyric Acid Derivatives, IR Spectra, NMR Spectra, X-Ray | | | |
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| default:Reihe_B/52/ZNB-1997-52b-0009.pdf | | | | Identifier
| ZNB-1997-52b-0009 | | | | Volume
| 52 | |
| 9 | Author
| R. Olf Minkwitz, Jens Jakob | Requires cookie* | | | Title
| Uber die Bildung von N,N-Bistrifluormethylhydroxylammoniumsalzen (CF3)2N(X)OX+MF6-(X = H, D; M = As, Sb) On the Formation o f N,N-Bistrifluoromethylhydroxylammonium Salts (CF3)2N(X)O X+MF6-(X = H, D; M = As, Sb) | | | | Abstract
| The preparation of the N,N-Bistrifluoromethylhydroxylammonium hexafluorometallates (CF3)2N(X)OX+MF6~ (X = H, D; M = As, Sb) is reported. The new compounds were cha racterized by IR, Raman, Mass, 'H , ,9F and l3C NM R spectroscopy. In addition we present our approach to the preparation of H-subsituted N,N-Bistrifluoromethylhydroxylammonium hexafluorometallates (C F ^ N (Y)O H +M F6~ (Y = C H 3, Cl, F; M = As, Sb). | | | |
Reference
| Z. Naturforsch. 52b, 958—964 (1997); eingegangen am 12. Mai 1997 | | | |
Published
| 1997 | | | |
Keywords
| N, N-Bistrifluoromethylhydroxylammonium Hexafluoroarsenate, N, N-Bistrifluoromethylhydr-oxylammonium Hexafluoroantimonate, Vibrational Spectra, NMR Spectra, Mass Spectra | | | |
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| default:Reihe_B/52/ZNB-1997-52b-0958.pdf | | | | Identifier
| ZNB-1997-52b-0958 | | | | Volume
| 52 | |
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