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. 94. Untersuchungen über Trithioallophansäure 3. Ester der Trithioallophansäure [1]

On Chalcogenolates. 94. Studies on Trithioallophanic Acid. 3. Esters of Trithioallophanic Acid. The esters of trithioallophanic acid H₂N? CS? NH? CS(SR) with R = CH₃, CH₂C₆H₅ have been characterized by means of electron absorption spectra, infrared spectra, ¹H NMR spectra, and mass spectra.     

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. 89. Untersuchungen über N-Dicyandithiocarbamidsäure Darstellung und Eigenschaften der freien Säure

On Chalcogenolates. 89. Studies on N-Dicyandithiocarbamic Acid. Preparation and Properties of the Free Acid Colorless N-dicyandithiocarbamic acid (melting point: 112°C) has been prepared by reaction between a suspension of K[S₂C? N(CN)₂] in diethyl ether and a solution of HCl in (C₂H₅)₂O at 0°C; the ether was distilled off at 0°C in vacuo. The compound has been characterized by means of infared spectra, electron absorption spectra, ¹H-NMR spectra, and mass spectra. The dissociation constant of N-dicyandithiocarbamic acid in water is K_a = (1.69 ± 0.1) X 10^?1 20°C. The thermodynamic data of the dissociation were calculated.     

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. 153. Untersuchungen über Derivate der N-Thioformyldithiocarbamidsäure 3. Ester der N-Thioformyldithiocarbamidsäure und Oxydation von N-Thioformyldithiocarbamaten

On Chalcogenolates. 153. Studies on Derivatives of N-Thioformyl Dithiocarbamic Acid. 3. Esters of N-Thioformyl Dithiocarbamic Acid and Oxidation of N-Thioformyl Dithiocarbamates The esters of N-thioformyl dithiocarbamic acid have been prepared by reaction of tetra-n-butylammonium N-thioformyl dithiocarbamate with the corresponding alkyl iodide. Also the reaction of S-methyl N-formyl dithiocarbamate with Lawesson reagent forms the methyl ester of N-thioformyl dithiocarbamic acid. The oxidation of N-thioformyl dithiocarbamates with iodine yields 1,2,4-dithiazole-3-thione All compounds have been characterized by means of chemical and diverse spectroscopic methods. A new method to prepare 5-phenyl 1,2,4-dithiazole-3-thione is given.     

Über Chalkogenolate. 105. Untersuchungen über Guanidinodithioformiate. 1. Darstellung und Eigenschaften von Guanidinodithioameisensäure

On Chalcogenolates. 105. Studies on Guanidinodithioformates. 1. Synthesis and Properties of Guanidinodithioformic Acid Yellow guanidinodithioformic acid has been prepared by reaction of guanidinium guanidinodithioformate in aqueous solution with concentrated hydrochloric acid at 0°C and characterized by diverse methods.     

Über Chalkogenolate. 82 [1]. N-Hydroxycarbamate und Ester der N-Hydroxycarbamidsäure und -carbimidsäure

On Chalcogenolates. 82. N-Hydroxy Carbamates and Esters of N-Hydroxy Carbamic Acid and Carbamic Acid The reaction between hydroxylammonium chloride, CO₂, and the corresponding hydroxide leads to N-hydroxy carbamates Esters of N-hydroxy carbamic acid have been prepared by reaction of N-hydroxy carbamates with alkyl bromide. – At room temperature the ethyl ester decomposes and forms the ester of N-hydroxy carbimic acid HO? N?C(OC₂H₅)₂. The prepared compounds have been characterized by different 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.     

Methylenverbindungen von Nichtmetallen. VI. Amide der Methan-bis(phosphonigsäure), -bis(phosphonsäure) und -bis(thiophosphonsäure)

Methylene Compounds of Non-Metals. VI. Amides of Methane-bis(phosphonous Acid), -bis(phosphonic Acid) and -bis(thiophosphonic Acid) Symmetrical- and asymmetrical-substituted amides of methane-bis(phosphonous acid), -bis(phosphonic acid) and -bis(thiophosphonic acid) have been obtained by stepwise aminolysis of the chlorides Cl₂(Z)PCH₂P(Z)Cl₂ ( 1 : Z = electron pair; 7 : Z = S; 13 : Z = O) and the fluoride F₂(S)PCH₂P(S)F₂ 19 with dimethylaminotrimethylsilane. Oxidation reactions of trivalent phosphonous amides with sulfur and dimethylsulfoxide have also been investigated.     

Über Chalkogenolate. 175. Reaktion von Acetamidin mit Kohlenstoffdisulfid 4. Darstellung und Charakterisierung der N-Acetimidoyldithiocarbamidsäure

On Chalcogenolates. 175. Reaction of Acetamidine with Carbon Disulfide. 4. Synthesis and Characterization of N-Acetimidoyl Dithiocarbamic Acid Orange colored N-acetimidoyl dithiocarbamic acid has been prepared by reaction of the acetimidinium salt in aqueous solution with hydrochloric acid at 0°C. The properties and the thermal behaviour of the acid have been described, its decomposition in solution has been studied at 20°C kinetically.     

Beiträge zur Kenntnis des chromophoren Systems der Corrine. X. Über die Reaktion von Derivaten des Cobyrinsäure-heptamethylesters mit unterchloriger Säure

Contributions to the Knowledge of the Corrin Chromophore, X. Reaction of Derivatives of Cobyrinic Acid Heptamethyl Ester with Hypochlorous Acid (Cobalt)-dicyano-, chloro-cyano-, and dichloro-cobyrinic acid heptamethylesters ( 1, 2 and 3 ), respectively, as well as their 10-chloro derivatives 4, 5 and 6 react with hypochlorous acid. A report on the structure and some properties of the reaction products 8, 9 and 10 is given.     

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. 141. Untersuchungen über Trimethylsilylxanthogensäure. 1. Darstellung und Eigenschaften von Trimethylsilylxanthaten

On Chalcogenolates. 141. Studies on Trimethylsilyl Xanthic Acid. 1. Synthesis and Properties of Trimethylsilyl Xanthates The trimethylsilyl xanthates have been prepared by reaction of the corresponding silanolate with carbon disulfide. The compounds were characterized by means of chemical and diverse spectroscopic methods. The existence of unstable trimethylsilyl xanthic acid has been demonstrated.     

Über Chalkogenolate. 99. Untersuchungen über Monothiocarbamidsäure 1. Darstellung und Eigenschaften von Monothiocarbamaten

On Chalcogenolates. 99. Studies on Monothiocarbamic Acid. 1. Synthesis and Properties of Monothiocarbamates The monothiocarbamates , and Ba[SOC? NH₂]₂ have been prepared and characterized by means of infrared, electron absorption, and mass spectra. The existence of the free monothiocarbamic acid was ascertained.     

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. 117 [1]. Untersuchungen über Guanidinodithioformiate 4. Kristall- und Molekülstruktur der Guanidinodithioameisensäure

On Chalcogenolates. 117. Studies on Guanidinodithioformates. 4. Crystal and Molecular Structure of Guanidinodithioformic Acid Guanidinodithioformic acid crystallizes with Z = 4 in the monoclinic space group P2₁ with cell dimensions a = 4.204(3) Å, b = 10.422(5) Å, c = 12.491(5) Å, β = 93.9(3)°. The crystal and molecular structure has been determined from single crystal X-ray data at 20°C and refined to a conventional R of 0.0242. The asymmetric part of the unit cell contains two molecules in the dipolar form with different conformation. The molecules have delocated double-bonds and are linked together by N? H···S hydrogen bridges.     

Dreifach-Diamantstruktur von. 2,6-Dioxoadamantan-1,3,5,7-tetracarbonsäure (Hydrat) als Wirtsgitter für Essigsäure

Triple-Diamond Structure of 2,6-Dioxoadamantane-1,3,5,7-tetracarboxylic Acid (Hydrate) as Host Lattice for Acetic Acid A novel solid-state channel-inclusion compound characterized by X-ray methods is based on three interpenetrating, translationally equivalent super-diamond network as host structure and AcOH as guest. The diamondoid host network are fromed by the 2,6-dioxoadamantane-1,3,5,7-tetracarboxylic acid tied together via pairwise H-bonds. The channels embedding the AcOH molecules may be viewed as symmetric triple helices winding about the guest species. Prospects regarding design and potentialities of diamondoid inclusion compounds are exemplified and appear promising.     

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. 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.