Über Chalkogenolate. 93. Untersuchungen über Trithioallophansäure 2. Darstellung und Eigenschaften der freien Säure [1]

On Chalcogenolates. 93. Studies on Trithioallophanic Acid 2. Preparation and Properties of the Free Acid Yellow trithioallophanic acid H₂N? CS? NH? CS(SH) has been prepared by reaction between a suspension of K[S₂C? NH? CS? NH₂] in diethyl ether and a solution of HCl in (C₂H₅)₂O at ?15°C; the ether was distilled off at ?15°C in vacuo. The compound has been characterized by means of infrared spectra, electron absorption, ¹H-NMR spectra, and mass spectra. The dissociation constant of trithioallophanic acid in water is K_a = (1,41 ± 0,08) · 10^?2 at 20°C.     

Über Chalkogenolate. 92. Untersuchungen über Trithioallophansäure 1. Alkalimetalltrithioallophanate

On Chalcogenolates. 92. Studies on Trithioallophanic Acid 1. Trithioallophanates of Alkali Metals The trithioallophanates have been prepared by reaction of H₂S with the corresponding dithiocarbimate. The compounds have been characterized by different methods. In aqueous solution the equivalent conductivites of [S₂C? NH? CS? NH₂]^? have been determined by means of conductivity measurements. The Stokes radius of the ion, the radius of the hydrated ion, and its diffusion coefficient were calculated.     

Über Chalkogenolate. 81. Untersuchungen über N-Hydroxydithiocarbamidsäure 3. Ester der N-Hydroxydithiocarbimidsäure und -carbamidsäure

On Chalcogenolates. 81. Studies on N-Hydroxy Dithiocarbamic Acid. 3- Esters of N-Hydroxy Dithiocarbimic Acid and Dithiocarbamic Acid The reaction between hydroxylamine, carbon disulfide, and alkyl halide leads to the corresponding ester of N-hydroxy dithiocarbimic acid HO? N?C(SR)₂ with R = CH₃, C₂H₅; R₂ = ? CH₂? CH₂? . The phenyl ester of N-hydroxy dithiocarbamic acid HO? NH? CS(SC₆H₅) has been prepared by reaction of hydroxylammonium chloride with the phenyl ester of chlorodithioformic acid. N-Methyl hydroxylammonium chloride reacts with carbon disulfide and alkyl iodide to form the corresponding ester of the dithiocarbamic acid HO? N(CH₃)? CS(SR) with R = CH₃, C₂H₅. The unstable compounds have been characterized by different methods.     

Über Chalkogenolate. 142. Untersuchungen über Trimethylsilylxanthogensäure. 2. S-Methyl- und S-Ethyltrimethylsilylxanthat

On Chalcogenolates. 142. Studies on Trimethylsilyl Xanthic Acid. 2. S-Methyl and S-Ethyl Trimethylsilyl Xanthates The hitherto unknown S-alkyl trimethylsilyl xanthates (CH₃)₃SiO? CS? SR, where R = CH₃ and C₂H₅, have been characterized with electron absorption, infrared, nuclear magnetic resonance (¹H, ¹³C, and ²⁹Si), and mass spectra.     

Über Chalkogenolate. 85. Untersuchungen über Halbester der Trithiokohlensäure 3. Schwingungsspektren von Alkylthioxanthogensäuren und Wasserstoffbrücken in den freien Säuren

On Chalcogenolates. 85. Studies on Hemiesters of Trithiocarbonic Acid 3. Vibrational Spectra of Alkyl Thioxanthic Acids and Hydrogen Bondings in the Free Acids The IR spectra of alkyl thioxanthic acids RS? CS(SH) with R = CH₃, C₂H₅, ⁿC₃H₇, ⁱC₃H₇, ⁿC₄H₉, ^sC₄H₉, ^tC₄H₉, and CH₃S? CS(SD) as well as the Raman spectrum of the Compound with R = CH₃ have been assigned. The formation of hydrogen bondings in the free acids has been studied by means of i.r. spectra, ¹H-n.m.r. spectra, and electron absorption spectra. The energies of the hydrogen bondings have been calculated.     

Über Chalkogenolate. 151. Untersuchungen über Derivate der N-Thioformyldithiocarbamidsäure. 1. Darstellung und Eigenschaften von N-Thioformyldithiocarbamaten

On Chalcogenolates. 151. Studies on Derivatives of N-Thioformyl Dithiocarbamic Acid. 1. Synthesis and Properties of N-Thioformyl Dithiocarbamates The N-thioformyl dithiocarbamates M[S₂C? NH? CS? H], where M = K, Rb, Cs, Tl, NH₄, [N(ⁿC₄H₉)₄], Na[S₂C? NH? CS? H] · 0.5 H₂O, and Ba[S₂C? NH? CS? H]₂ · 3 HO? CH₂? CH₂? OCH₃ have been prepared by use of partial different procedures. The compounds were characterized with chemical and thermal methods as well as by means of electron absorption, infrared, nuclear magnetic resonance (¹H and ¹³C), and mass spectra. Attempts to synthesize N-thioformyl dithiocarbamic acid were not successful.     

Über Chalkogenolate. 156. Reaktion von N-Methylformamid mit Kohlenstoffdisulfid 3. Alkylester der N-Methyl-N-formyldithiocarbamidsäure

On Chalcogenolates. 156. Reaction of N-Methyl Formamide with Carbon Disulfide. 3. Alkyl Esters of N-Methyl N-Formyl Dithiocarbamic Acid The hitherto unknown esters of N-methyl N-formyl dithiocarbamic acid H? CO? NCH₃? CS? SR, where R = CH₃ and C₂H₅, have been characterized by means of electron absorption, infrared, nuclear magnetic resonance (¹H and ¹³C), and mass spectra.     

Über Chalkogenolate. 205. Reaktion von Acetamid mit Kohlenstoffdisulfid 2. Ester der N-Acetyldithiocarbamidsäure

On Chalcogenolates. 205. Reaction of Acetamide with Carbon Disulfide. 2. Esters of N-Acetyl Dithiocarbamic Acid The prepared yellow esters of N-acetyl dithiocarbamic acid H₃C? CO? NH? CS? SR with R = CH₃, C₂H₅ have been characterized by means of mass, electron absorption, infrared, and nuclear magnetic resonance spectra.     

Über Chalkogenolate. 203. Derivate der Selendithioallophansäure 2. Darstellung und Eigenschaften von Alkylestern

On Chalcogenolates. 203. Derivatives of Selenodithioallophanic Acid. 2. Preparation and Properties of Alkyl Esters Synthesis and properties of selenodithioallophanic acid esters H₂N? CSe? NH? CS? SR where R = CH₃, C₂H₅ as well as their characterization by means of electron absorption, infrared, and nuclear magnetic resonance spectra are described.     

Über Chalkogenolate. 122. Untersuchungen über N-Cyanomonothiocarbimidsäure 2. Kalium-S-methyl-N-cyanomonothiocarbimat und S-Methyl-N-cyanomonothiocarbimidsäure

On Chalcogenolates. 122. Studies on N-Cyanomonothiocarbimic Acid. 2. Potassium S-Methyl N-Cyanomonothiocarbimate and S-Methyl N-Cyanomonothiocarbimic Acid The reaction of K₂[SOC?N? CN] · H₂O with H₃CI gives K[O(H₃CS)C?N? CN]. The potassium salt reacts with acid to form (HO)(H₃CS)C?N? CN and with H₃CO? CO? Cl to yield (H₃CO? CO? O)(H₃CS)C?N? CN. The compounds have been characterized by means of spectroscopic methods.     

Über Chalkogenolate. 123. Untersuchungen über N-Cyanomonothiocarbimidsäure. 3. O,S-Dimethylester der N-Cyanomonothiocarbimidsäure. Thiolyse und Hydrolyse des Esters

On Chalcogenolates. 123. Studies on N-Cyanomonothiocarbimic Acid. 3. O, S-Dimethyl Ester of N-Cyanomonothiocarbimic Acid. Thiolysis and Hydrolysis of this Ester (H₃CO)(H₃CS)C?N? CN has been prepared by reaction of K₂[SOC?N? CN] · H₂O with H₃CI. The thiolysis of this ester gives (H₃CO)(H₃CS)C?N? CS? NH₂. The acid hydrolysis forms (H₃CO)(H₃CS)C?N? CO? NH₂ via [(H₃CO)(H₃CS)C?N? C?NH]Cl. All compounds have been characterized by diverse methods.     

Über Chalkogenolate. 100. Untersuchungen über Monothiocarbamidsäure. 2. S-Methyl- und O-Methylmonothiocarbamat, 2,4,5-Trioxo-thiazolidin-(1,3)

On Chalcogenolates. 100. Studies on Monothiocarbamic Acid. 2. S-Methyl and O-Methyl Monothiocarbamate, 2,4,5-Trioxo-thiazolidine-(1,3) The methyl esters of monothiocarbamic acid H₂N? CO? SCH₃ and H₂N? CS? OCH₃ as well as 2,4,5-trioxo-thiazolidine-(1,3) and its potassium salt have been prepared and characterized by means of electron absorption, infrared, ¹H-NMR, and mass spectra.     

Über Chalkogenolate. 150. Reaktion von Formamid mit Kohlenstoffdisulfid 4. Ester der N-Formyldithiocarbamidsäure

On Chalcogenolates. 150. Reaction of Formamide with Carbon Disulfide. 4. Esters of N-Formyl Dithiocarbamic Acid The hitherto unknown esters of N-formyl dithiocarbamic acid H? CO? NH? CS? SR, where R ? CH₃ and C₂H₅, have been characterized by means of diverse spectroscopic methods.     

Über Chalkogenolate. 134. Untersuchungen über Ester von Halogenoameisensäuren 2. Darstellung und Eigenschaften von Se-Alkylestern der Chloromonothiomonoselenoameisensäure [1]

On Chalcogenolates. 134. Studies on Esters of Haloformic Acids 2. Synthesis and Properties of Se-Alkyl Esters of Chloromonothiomonoselenoformic Acid The hitherto unknown esters RSe? CS? Cl with R ? C₂H₅ and ⁿC₃H₇ have been prepared by reaction of thiophosgene with the corresponding alkane selenol. The compounds have been characterized with electron absorption, nuclear magnetic resonance (¹H, ¹³C, and ⁷⁷Se), infrared, and mass spectra.     

Über Chalkogenolate. 95. Untersuchungen über Trithioallophansäure 4. Metall(I,II)- trithioallophanate

On Chalocogenolates. 95. Studies on Trithioallophanic Acid. 4. Metal(I, II) Trithioallophanates. The prepared trithioallophanates M[S₂C-NH-CS-NH₂] with M = TI, Ag well as M[S₂C-NH-CS-NH₂]₂ with M = Pb, Cu, Zn, Cd, Hg have been investigated by different methods.     

Über Chalkogenolate. 206 [1]. N-Thioacetyldithiocarbamate und Ester der N-Thioacetyldithiocarbamidsäure

On Chalcogenolates. 206. N-Thioacetyl Dithiocarbamates and Esters of N-Thioacetyl Dithiocarbamic Acid Thioacetamide reacts with carbon disulfide in the presence of KH to form via the tetrabutyl ammonium salt dark yellow N-thioacetyl dithiocarbamates M[S₂C? NH? CS? CH₃], where M = K, Rb, Cs. The salts as well as the methyl and ethyl ester have been characterized by means of electron absorption, infrared, nuclear magnetic resonance (¹H and ¹³C), and mass spectra. Attempts to synthesize N-thioacetyl dithiocarbamic acid were not successful.     

Über Chalkogenolate. 136 [1]. Alkylester der Cyanoameisensäure und der Cyanomonothioameisensäure

On Chalcogenolates. 136. Alkyl Esters of Cyanoformic Acid and of Cyanomonothioformic Acid By use of the phase transfer catalyst 18-crown-6 the esters CH₃O—CO—CN, C₂H₅O—CO—CN, C₂H₅S—CO—CN, and ⁿC₃H₇S—CO—CN have been prepared by reaction of the corresponding chloro compound with potassium cyanide. The prepared compounds have been characterized by means of electron absorption, infrared, nuclear magnetic resonance (¹H and ¹³C), and mass spectra.     

Über Chalkogenolate. 113 Umsetzung von Chloramin mit Kohlenstoffdisulfid und mit Methylestern von Dithiocarbamidsäuren

On Chalcogenolates. 113. Reactions of Chloramine with Carbon Disulfide and with Methylesters of Dithiocarbamic Acids The reactions of chloramine with CS₂ and with H₂N? CS? SCH₃, CH₃? NH? CS? SCH₃, and (CH₃)₂N? CS? SCH₃ have been studied. The reaction with the methylester of dithiocarbamic acid gives the known dimethyl perthiocyanate and the reaction with the methylester of N-methyldithiocarbamic acid leads to CH₃S? CS? N(CH₃)? C(?NCH₃)? SCH₃. The latter compound has been characterized by means of electron absorption spectra, infrared spectra, nuclear magnetic resonance spectra (¹H and ¹³C), and mass spectra.     

Raman und infrarotspektroskopische Untersuchungen an Alkylderivaten der Arsensäure. III. Die Schwingungsspektren von Methan- und Äthanarsonsäure sowie von Natriumhydrogenmethanarsonat

RAMAN and IR-spectroscopic Investigation of Alkyl Derivatives of Arsenic Acid. III. The Vibrational Spectra of Methane and Ethanearsonic Acid and Sodium Hydrogenmethanearsonate. The RAMAN spectra of CH₃AsO₃H₂, C₂H₅AsO₃H₂ CH₃AsO₃HN₂. 3/2 H₂O (solid and in concentrated aqueous solution) and the IR spectra (400 -4000 cm^?1) of these solid acids – partially deuterated – and of the hydrogenarsonate are discussed. The very probable symmetry of these compounds is C_s. As the IR spectra show (two strong broad OH valence bands at 2820 and 2350 cm^?1; OH deformation frequency at 1220 cm^?1), rather strong H-bonds exist in these acid substances.     

Über Chalkogenolate. 160. Umsetzung von 1,2-Ethandithiolaten mit Kohlenstoffdisulfid 2. 1,2-Ethan-bis(trithiokohlensäure) und Alkylester der Säure

On Chalcogenolates. 160. Reaction of 1,2-Ethanedithiolates with Carbon Disulfide. 2. 1,2-Ethane-bis(trithiocarbonic acid) and Alkyl Esters of This Acid The reaction of potassium 1,2-ethane-bis(trithiocarbonate) with hydrochloric acid at 0°C gives unstable, deep yellow coloured 1,2-ethane-bis(trithiocarbonic acid) The 1,2-ethane-bis(alkyl trithiocarbonates) RS? CS? SCH₂CH₂S? CS? SR, where R = CH₃ and C₂H₅, have been formed by reaction of potassium 1,2-ethane-bis(trithiocarbonate) with the corresponding alkyl iodide. The called compounds have been characterized by means of diverse spectroscopic methods.