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  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 406 (1974), S. 167-170 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation of LiAl[P(CH3)2]4 and Silylphosphines H3-x(CH3)xSi—P(CH3)2By metallation of HP(CH3)2 with LiC4H9 (in diglyme, at -40°C) and the subsequent reaction of the LiP(CH3)2 with AlCl3 the compound LiAl[P(CH3)2]4 is obtained (solution in diglyme). The reactions with H3SiBr, CH3SiH2Br, (CH3(2)SiHBr, and (CH3)3)SiCl results in the formation of H3SiP(CH3)2, CH3SiH2,—P(CH32, (CH3)2)SiHP(CH3)2, and (CH3)3Si—P(CH3)2 in large quantities.
    Notes: Durch Metallierung von HP(CH3)2 mit LiC4H9 in Diglym bei -40°C und anschließende Umsetzung des gebildeten LiP(CH3)2 mit AlCl3 wird das LiAl[P(CH3)2]4 zugänglich (Lösung in Diglym). Die Umsetzung mit H3SiBr, CH3SiH2Br, (CH3)2SiHBr und (CH3)3SiCl führt zur präparativen Darstellung von H3Si—P(CH3)2, CH3SiH2—P(CH3)2, (CH3)2SiH—P(CH3)2 (CH3)3Si—P(CH3)2.
    Additional Material: 1 Ill.
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 407 (1974), S. 295-304 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation of Silylphosphines of the X3-(n+m)(CH3)nHmSi—PH2 Type (X = F, Cl, Br)Reactions of halosilanes with silylphosphines containing PH2-groups are reported. CH3SiHCl—PH2 is obtained by (1) For the synthesis of Cl3Si—PH2 reactions of SiCl4 with CH3SiH(PH2)2, CH3SiH2—PH2 and (CH3)3Si—PH2 are carried out in a manner analogous to that shown in eq. (2) Side reactions are observed. Cl3Si—PH2 is isolated in mixture with SiCl4 and CH3SiHCl—PH2 when the most reactive of the above compounds, CH3SiH(PH2)2 is utilized.
    Notes: Es wird über Reaktionen zwischen Halogensilanen und PH2-haltigen Silylphosphinen berichtet. CH3SiHCl—PH2 wird nach Gl. (1) zugänglich. Zur Bildung von Cl3Si—PH2 wurden Umsetzungen von SiCl4 mit CH3SiH(PH2)2, CH3SiH2—PH2 und (CH3)3Si—PH2 durchgeführt, wobei Reaktionen entsprechend Gl. (2) eintreten. Es treten Nebenreaktionen auf. Beim reaktionsfähigeren CH3SiH(PH2)2 ist die Isolierung von Cl3Si—PH2 im Gemisch mit SiCl4 und CH3SiHCl—PH2 möglich. Unter den Reaktionsbedingungen (50°C) zerfällt Cl3Si—PH2 in PH3 und Si—P-Polymere. SiBr4 reagiert bereits bei Raumtemperatur. Durch Umsetzung mit CH3SiH(PH2)2 werden je nach Reaktionsdauer CH3SiHBr—PH2, Br3Si—PH2 und auch Br2Si(PH2)2 zugänglich. Auch die Reaktion mit CH3SiH2—PH2 führt zum Br3Si—PH2 neben CH3SiH2Br. Mit FSiBr3 bildet CH3SiH(PH2)2 das FSiBr2—PH2 neben CH3SiHBr—PH2, während bei den F-reicheren Derivaten F2SiBr2 und F3SiBr die Disproportionierung in SiF4 gegenüber der Si—P-Spaltung überwiegt. Es werden die NMR-Daten der Verbindungen angegeben.Cl3Si—PH2 decomposes into PH3 and Si—P-polymers under the reaction conditions (50°C). SiBr4 however will react at room temperature. Depending on the time of reaction CH3SiHBr—PH2, Br3Si—PH2 and even Br2Si(PH2)2 are obtained with CH3SiH(PH2)2. Also the reaction with CH3SiH2—PH2 leads to the formation of Br3Si—PH2 in addition to CH3SiH2Br. With FSiBr3, CH3SiH(PH2)2 forms FSiBr2—PH2 together with CH3SiHBr—PH2. In the reaction of the higher fluorinated derivatives F2SiBr2 and F3SiBr the disproportion into SiF4 is found to be preferred to Si—P cleavage and therefore these reactions can not be adequately used. The nmr data are reported.
    Additional Material: 3 Tab.
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 409 (1974), S. 137-151 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: NMR Studies on Silylphosphines. II. Effects of Substituents in Silyl- and SilylmethylphosphinesThe influence of the substituents [CH3, H, H3Si, (CH3)3Si] on: chemical shifts of protons and phosphorus nuclei: the 29Si-31P coupling constant; and several proton coupling constants in the nmr spectra of 24 silylphosphines of the series (CH3)xH3-x,Si-PH2, (CH3)xH3-xSi-PHCH3, (CH3)xH3-xSi-P(CH3)2, [(CH3)xH3-xSi]2PH, [(CH3)xH3-xSi]2PCH3, [(CH3)xH3-x,Si]3P has been studied. Empirical methods for the calculation of δ31P and J29Si-31P using bond increments are reported.
    Notes: Es wird der Einfluß der Substituenten [CH3, H, H3Si, (CH3)3Si] auf die chemische Verschiebung der Protonen und der Phosphorkerne sowie auf die 29Si-31P-Kopplungskonstante und auf einige Protonenkopplungen in 24 Silylphosphinen der Gruppen (CH3)xH3-x,Si-PH2, (CH3)xH3-xSi-PHCH3, (CH3)xH3-xSi-P(CH3)2, [(CH3)xH3-xSi]2PH, [(CH3)xH3-xSi]2PCH3, [(CH3)xH3-x,Si]3P anhand der NMR-Spektren untersucht. Es werden empirische Verfahren zur Berechnung von δ31 und J29Si-31P aus Bindungsinkrementen mitgeteilt.
    Additional Material: 6 Ill.
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  • 4
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Journal für Praktische Chemie/Chemiker-Zeitung 316 (1974), S. 19-25 
    ISSN: 0021-8383
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 2-Aryl-4-amino-5-benzoyl-thiazole 2 werden zu 2-Aryl-4-acylamino-5-benzoyl-thiazolen 4 acyliert und in Form ihrer Perchlorate 3 mit Ketomethylenverbindungen bzw. Säureamid-Derivaten zu Thiazolo[4,5-b]pyridinen 5 bzw. Thiazolo[4,5-d]pyrimidinen 6 umgesetzt.
    Additional Material: 3 Tab.
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  • 5
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Journal für Praktische Chemie/Chemiker-Zeitung 322 (1980), S. 87-93 
    ISSN: 0021-8383
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis and Reactions of 2-Arylazo-2-nitro-keten AminalsN,N′-Disubstituted 1-nitro-2,2-diamino ethylenes 1 undergo azo-coupling to form the title compounds 2. Their treatment with oxalyl chloride yields the imidazolidin-4,5-dione-derivatives 4. 2 react with phosgene and thiophosgene to form 6-nitro-2,4-diaryl-5-arylimino-2,3,4,5-tetrahydro-1,2,4-triazin-3-ones 5 and -thiones 6 respectively. From 2 and N-(dichloromethylene)-arylsulfoamides the 6-nitro-2,4-diaryl-5-arylimino-3-aryl-sulfonylimino-2,3,4,5-tetrahydro-1,2,4-triazines 7 arise. The reduction of 2 yields the substituted oxalic amidines 9
    Additional Material: 2 Tab.
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  • 6
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Journal für Praktische Chemie/Chemiker-Zeitung 315 (1973), S. 44-46 
    ISSN: 0021-8383
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Cyanamid reagiert mit Mandelsäurenitril und Benzaldehyd zum 2-Amino-5-cyan-4,5-diphenyl-Δ2-oxazolin 1, das in Gegenwart von Basen einer Eliminierung zu 2-Amino-4,5-diphenyl-oxazol 2 unterliegt und säurekatalysiert zum 2-Amino-5-cyan-4,5-diphenyl-oxazolidinon 4 hydrolysiert wird.
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  • 7
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Journal für Praktische Chemie/Chemiker-Zeitung 315 (1973), S. 497-504 
    ISSN: 0021-8383
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Durch Umsetzung von 2-arylsubstituierten 1,3-Oxathioliumsalzen 1 mit CH-aciden Nitrilen und Estern sowie Cyanamid lassen sich 3-Amino- bzw. 3-Hydroxythiophene 9, 11, 12 sowie 4-Aminothiazole 10 gewinnen, deren Struktur anhand spektroskopischer Daten bewiesen wird.
    Additional Material: 3 Tab.
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  • 8
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Journal für Praktische Chemie/Chemiker-Zeitung 316 (1974), S. 169-172 
    ISSN: 0021-8383
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Tab.
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  • 9
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Journal für Praktische Chemie/Chemiker-Zeitung 323 (1981), S. 133-136 
    ISSN: 0021-8383
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Methyl(3-amino-5-nitromethylene-1,2-dithiol-4)carboxylate
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  • 10
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Journal für Praktische Chemie/Chemiker-Zeitung 325 (1983), S. 41-48 
    ISSN: 0021-8383
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 3-Nitromethyl-pyrazoles from 2-Cyano-3-methylthio-4-nitrocrotonic Acid Derivatives2-Cyano-3-methylthio-4-nitrocrotonic Acid Derivatives 1a, b react with hydrazines to form the 5-amino-3-nitromethyl-pyrazoles 2a-c and the 5-nitromethyl-pyrazol-3-one 3 respectively. Contrary to this carboxylic hydrazides attacks the nitro group. For the resulting products the structure of pyrrol-2,5-dione oximes 4 is proposed. On the similar way from 3-methylthio-4-nitro-2-phenylcrotononitrile 1c and phenylhydrazine the pyrrol-2,5-dione hydrazone 5 arises. Subsequent reactions of 2 yield 3-nitromethyl-pyrazole derivatives 6, 3-nitromethyl-azinones 8 and nitromethyl-pyrazolyl-azo compounds 10.
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