Synthese neuer Indolderivate

The synthesis of the ,-unsaturated ketones4, 5 und6 via the regiospecific aldol- andWittigreaction with some indolealdehydes is described.4 and5 are stable enough for NaBH₄-reduction to the corresponding alcohols.

     

Synthese neuer Nonafulvene

Synthesis of New Nonafulvenes Nonafulvenes 1c and 1m – s are prepared by the following methods: (a) Elimination of AcOH from acetoxyalkyl-cyclononatetraenes (Scheme 2; 1m ); (b) alkylation of nonafulvenolates (Scheme 3; 1c , 1n ); (c) elimination of alcohol from di- and trialkoxymethyl-cyclononatetraenes (Scheme 5; 1o , 1p , 1q ); (d) deprotonation of intermediary formed formamidiniumcyclononatetraenes (Scheme 6; 1r , 1s ). Scope and limitations of these preparative sequences are discussed and compared with the corresponding pentafulvene syntheses.     

Synthese neuer organoelementsubstituierter pentadiene (1)

By applying four different methods twelve new organoelement substituted pentadienes have been prepared. They contain one or two organoelement groups. - Pentadienyllithium (2) reacted with Cl-SPh, Br-SePh, Cl-PPh₂, and Cl-AsPh₂ (lone pair at the element) exclusively to the corresponding E-1-(organoelement)-2,4-pentadiene, whereas with Cl-MMe₃ (M = Si, Ge, Sn) (2,3,4), Cl-GePh₃, and Cl-SnPh₃ (no lone pair at the element) a mixture of the E- and Z-1-(organoelement)-2,4-pentadiene is formed. An interpretation of this different behaviour is given.     

Synthese und spektroskopische Eigenschaften neuer komplexierter Triphosphane

Synthesis and Spectroscopy of new Triphosphine Complexes The reaction of PCl₃ with [HPPh₂W(CO)₅] in the presence of NEt₃ affords stepwise the diand triphosphine complexes [Cl₂PPPh₂W(CO)₅] and ClP[PPh₂W(CO)₅]. Triphosphine complexes of the type [{M′(CO)₅}(H)P{PPh₂M(CO)₅}] (M = M′ = Cr or Mo) are not formed from the reaction of HP[PPh₂M(CO)₅] with [M′(CO)₅thf]. However they were prepared by reaction of [M′(CO)₅PCl₃] with Li[PPh₂M(CO)₅]. The products were characterized by NMR, IR spectroscopy, and mass spectrometry.     

Synthese neuer 4-Hydroxybenzonitrilderivate und deren herbizide Eigenschaften

The synthesis of several new derivatives of 2-amino-4-hydroxybenzonitrile2 and their herbicidal screening data are described. Thus, halogenation and furtherSandmeyer-Reaction of2 leads to the 2,3,5-trihalogenated derivatives5 a–e. Reaction of ethyl chloroformate with the amino group of2 gives6 a, acylation7 a, b and8. The 3,5-dihalogenated compounds10 a–e are obtained from6 a and7 a, b by bromination or iodation. The hydroxyl group of6 a, 7 a, b and10 a, c, e reacts with N,N-disubstituted carbamyl chlorides to give6 c, d, 9 a, b, 11, 12 and13 a, b.

     

Synthese neuer mono- und dihalogenierter Salicylsäurederivate

Syntheses of 3- and 4-monohalogenated (2a, b; 3a–c; 4a–e) and 3,4-dihalogenated (4f–l) ethyl 5-cyano-salicylates are described. Nitration of the ethyl 5-cyano-4-halo-salicylates3a, b leads to the ethyl 5-cyano-4-halo-3-nitro-salicylates5a, b. Hydrolysis of the ester and cyano group as well as reactions of various chloroformates, N,N-dimethylcarbamyl chloride and acetic anhydride with the hydroxyl group have been studied.

     

Synthese und Charakterisierung neuer Acetylenkomplexe des Mangans und Rheniums

The reaction of the photochemically-generated tetrahydrofuran complexes Cp′(CO)₂M(thf) (Cp′  η⁵-C₅H₅, η⁵-C₅H₄Me, η⁵-C₅Me₅; M  Mn, Re) with various alkynes R¹C₂R² (R¹, R²  H, Me, Ph) yields are acetylene complexes Cp′(CO)₂MR¹C₂R². These compounds were identified from their IR, ¹H NMR, ¹³C NMR and mas spectra.     

Synthese und NMR-spektroskopische Charakterisierung neuer Adenin- und 6-Thioxopurincarboxamidine

Synthesis and NMR-Spectroscopic Characterization of New Adenine- and 6-Thioxopurinecarboxamidines Adenine (1) or 1H-purine-6(7H)-thione ( 4 ) react with carboximidoyl chlorides 2 to yield the adenine-9-carboxamidines 3 or the 6,7-dihydro-6-thioxo-1H-purine-7-carboxamidines 5 and 6,9-dihydro-6-thioxo-1H-purine-9-carboxamidine 6 a , respectively. The structures of the compounds were determined by ¹H- and ¹³C-NMR spectroscopy.     

Synthese neuer `Push‐Pull'‐Enine

Synthesis of Novel `Push‐Pull'‐Enynes `Push‐pull' enynes 14a – d with EtO, PhO, PhS, and MeS groups as π‐donors have been synthesized by catalyzed coupling of stannyl ynamines 10 with 3‐iodoprop‐2‐enal (Scheme 4).     

Über die Synthese neuer Pyrrol-2-carbonsäureamide

The preparation of 3-hydroxy-5-phenyl-pyrrol-2-carboxamides and their methylation and acetylation are described.     

Synthese und Charakterisierung neuer Cyclischer und acyclischer Silachalkogenane mit Disilanyleinheiten

Synthesis and Characterization of New Cyclic and Acyclic Silachalcogenanes with Disilanyl Units Synthesis and properties of (4-CH₃? C₆H₄)₃SiSiH₃, (C₆H₅)₂HSiSiH₂C₆H₅, C₆H₅Cl₂SiSiH₃, (C₆H₅)₂ClSiSiH₃, (H₃SiSiH₂)₂Se, H₃SiSiH₂ESiH₃, , as well as characterisation by IR-, MS-, NMR-spectroscopy are described. Reactions of phenylsubstituted disilanes with HCl in the presence of catalytic amounts of AlCl₃ provide chorinated chlorophenylsubstituted disilanes. Condensation of these chlorodisilanes with disilathiane or disilaselenane yield cyclic and acyclic silachalkogenanes containing disilanyl units. The structure of (C₆H₅)₃SiSiH₃ has been determined by X-ray analysis. The compound crystallizes in space group C2/c with the cell dimensions a = 16.366(2), b = 11.458(1), c = 19.719(2) Å, β = 110.93(1)°.