Über Phosphorstickstoffverbindungen. XXXIII. Reaktionen von Diphenyltrichlorphosphoran mit Hydraziniumsalzen und -derivaten

Hydrazinium monochloride disproportionates on interaction with diphenyl-trichlorophosphorane, giving N₂ and [(C₆H₅)₂P(Cl)? N? PCl(C₆H₅)₂]Cl. The phosphinazine dihydrochloride [(C₆H₅)₂PCl? NH? NH? PCl(C₆H₅)₂]Cl₂ is obtained according to equation (4). The preparation of the P? N five-ring compound X, formulated in ?Inhaltsübersicht”?, is described.     

Über Phosphorstickstoffverbindungen,XXXII. Über Vier- und fünfgliedrige Heterocyclen mit Phosphor,Stickstoff und Kohlenstoff im Ring

On reacting of oxamide with PCl₅ the syntheses of the new N-, C- and pentavalent phosphorus containing heterocycles I and II (see “Inhaltsübersicht”), built up from interconnected four- and fivemembered ring systems, have been achieved. Reaction of N, N′- dimethyloxamide with PCl₃ yields the compound III which may be chlorinated to IV. An intermolecular reaction between the PCl₃- and carbonyl groups of IV gives V. The fivemembered ring systems III and V may each be linked together via N? CH₃ bridges, i. e. via P? N(CH₃)? P and P(O)? N(CH₃)? P(O) units, respectively. N, N′- dimethyloxamide reacts with PCl₅ to form a mixture of fivemembered heterocycles containing trivalent phosphorus (as a PCl group) and chlorinated carbon.     

Über Reaktionen des P4S10 mit siliciumorganischen Verbindungen

Reactions of P₄S₁₀ with Organosilicon Compounds P₄S₁₀ ( 1 ) can be degraded with silicon-nitrogen compounds. 1 reacts with (CH₃)₃Si? N(CH₃)₂ ( 2 a ) and (CH₃)₃Si? N(C₂H₅)₂ ( 2 b ) to yield S?P[N(CH₃)₂]₂SSi(CH₃)₃ ( 3 a ) and ( 3 b ). By the reaction of 1 with [(CH₃)₃Si]₂S ( 4 ) S?P[S? Si(CH₃)₃]₃ ( 6 ) is formed in high yield. (C₆H₅PS₂)₂ ( 7 ) was used as a model to investigate the course of the reaction. This leads to C₆H₅P(S)? [N(CH₃)₂]SSi(CH₃)₃ ( 9 ) and C₆H₅P(S)[SSi(CH₃)₃]₂ ( 10 ). The reaction mechanism will be discussed. The n.m.r. data and mass spectra are reported.     

Zur Analyse von Halogene oder Stickstoff enthaltenden organischen Verbindungen

Ohne Zusammenfassung     

Über Phosphorstickstoffverbindungen. XXX. Ein neues fünfgliedriges Ringsystem mit Stickstoff,Phosphor und Kohlenstoff im Ring

Diphenylthiosemicarbazide reacts with PCl₃ to form the fivemembered cyclic system Ia (see ”?Inhaltsübersicht?), whereas with PCl₅ the compound II is formed. With PCl₅ Ib is formed from Ia, with Cl₂ II.     

Über Phosphorstickstoff-Verbindungen XXVIII. Über Reaktionen von Cyanamid,Dicyanimid und Dicyandiamid mit PCl5

Interaction between cyanamide and PCl₅ in the mole ratio 1:3 yields the phosphazenium salt [Cl₃P?N? C(Cl)?N? PCl₃] [PCl₆]. The reaction of sodium dicyanimide and PCl₅ gives 1. 1. 3. 5-tetrachloro-1-phospha-2. 4. 6-triazine (compound B in ?Inhaltsübersicht”?). Dicyandiamide and PCl₅ (1:2) give compound C and, at milder conditions the salt-like phosphatriazine D. Solvolysis of C with formic acid or of D with sulphur dioxide yields E.     

Über einige neue Verbindungen von Stickstoff und Wasserstoff mit Metallen

Ohne Zusammenfassung     

über Verbindungen des Thoriums mit Stickstoff und Wasserstoff

Preparation and Vibrational Spectra of N-Trimethylsilyl-Tris(trimethylsiloxy)-Vanadium (V) imine, (Me₃SiO)₃V?N? SiMe₃ The preparation of the title compound from VOCl₃ and hexamethyl-disilazane is described. The vibrational spectra of the compound suggest a vanadium-nitrogen triple bond and a near linear vanadium–nitrogen–silicon arrangement.     

Über fluoreszierende Verbindungen von Kupfer(I)-jodid mit aromatischen Stickstoffbasen

On Fluorescent Compounds of Copper(I) Iodide with Aromatic Nitrogenous Bases The easily obtainable compounds of copper(I) iodide with esters of nicotinic acid, with nicotinic acid amide and nitrile, as well as with quinoline, isoquinoline and quinaldine are strongly fluorescent in ultraviolet light. They are remarkably stable against water and air, compared with analogous picoline and lutidine compounds. Only in one case (nicotinic acid hexyl ester-copper(I) iodide) the phenomenon of fluorescence thermochromism has been observed.     

Über Phosphorstickstoff-Verbindungen. XXXI. Über neue viergliedrige Ringsysteme mit Stickstoff,Phosphor und Kohlenstoff im Ring

A P? N compound XI, formula see ?Inhaltsübersicht”?, has been prepared containing three interconnected four-membered rings. On chlorination of XI P₂(NCH₃)₂Cl₆ is re-formed, besides a further product being very probably compound XII with hexa-coordinated phosphorus. Interaction between the known Cl₄P(NCH₃)₂ CCl₂ and NN′-dimethyl urea yields III and another compound, VII, with phosphorous of coordination number six.     

Zur Absorption von Stickstoff und Stickstoff enthaltenden Gasen

Ohne Zusammenfassung     

Über Reaktionen von Antimonhalogeniden. II. Die Reaktion von SbCl5 mit Oxalsäure-bis-(methylamid)

Reactions of Antimony Halides. II. The Reaction of SbCl₅ with Oxalic Acid Bis(methylamide) The reaction of antimony pentachloride with the dimethylamide of oxalic acid results in the formation of a five-ring heterocyclic compound C₄H₇Cl₄N₂O₂Sb(I), in which the ring components are Sb, N, C and O. It's synthesis and properties are discussed. Results of the mass spectrum see Table 1, a fraction scheme is given.     

Über thermische,eine Amino-Claisen-Umlagerung einschliessende. Reaktionen von N-Propargyl-naphthylaminen

N-Propargyl-1-naphthylamine ( 1 ), the corresponding N-butinylcompound 5 and N-propargyl-2-naphthylamine ( 2 ) - unlike N-propargyl-anilines - on heating to 250° are converted to a mixture of py-tetrahydro-benzoquinolines and benzoquinolines (scheme 1). The mechanism of these reactions which are induced by a [3s, 3 s] rearrangement of the propargyl group and include a [1,5s] H-shift is depicted in scheme 4. N-Methylation of 1 and 2 reduces for steric reasons the rate of the [1,5s] H-shifts; therefore ring closure of the allenylnaphthylamine intermediates to indols 13 and 14 is favoured (schemes 2 and 5).