Thion‐ und Dithioester, XXIV. Synthese von Tetrathiooxalestern

Hartke, Klaus; Kissel, Thomas; Quante, J.; Matusch, Rudolf

doi:10.1002/cber.19801130525

Cited by 140 publications

(31 citation statements)

References 17 publications

(1 reference statement)

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“…Deuterated (98%) bis(ethylenedithiolo)-tetrathiofulvalene (D8-ET) was grown according to Hartke et al [69] and Mizumo et al [70], making the reduction of carbon disulfide with potassium in dimethylformamide and subsequent reaction with deuterated (98%) 1.2-dibromoethane. The intermediate thione C 5 D 4 S 5 was mixed with triethylphosphite in an inert atmosphere kept at 1200…”

Section: Sample Preparationmentioning

confidence: 99%

Probing the Mott physics inκ-(BEDT-TTF)₂X salts via thermal expansion

Souza

Bartosch

2015

J. Phys.: Condens. Matter

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In the field of interacting electron systems the Mott metal-to-insulator (MI) transition represents one of the pivotal issues. The role played by lattice degrees of freedom for the Mott MI transition and the Mott criticality in a variety of materials are current topics under debate. In this context, molecular conductors of the κ-(BEDT-TTF) 2 X type constitute a class of materials for unraveling several aspects of the Mott physics. In this review, we present a synopsis of literature results with focus on recent expansivity measurements probing the Mott MI transition in this class of materials. Progress in the description of the Mott critical behavior is also addressed.

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Section: Sample Preparationmentioning

confidence: 99%

Probing the Mott physics inκ-(BEDT-TTF)₂X salts via thermal expansion

Souza

Bartosch

2015

J. Phys.: Condens. Matter

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“…Metastable analysis indicates that the elimination of CO from the molecular ion constitutes the main fragmentation channel, in good 64 (3) 64 (8) 64 (7) 64 (9) 64 (9) [CHZS,l+' "Only peaks above mlr 50 and greater than 2% relative abundance are included.…”

Section: Resultsmentioning

confidence: 99%

Mass spectrometry in isomer differentiation: 4,5‐bis(alkylthio)‐1,3‐dithiol‐2‐ones and 1,2‐dithiol‐3‐ones

Andreu

Gayán

Garı́n

et al. 1994

Rapid Comm Mass Spectrometry

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A mass spectrometric study of compounds 1 seemed worthwhile for two reasons: (i) to our knowledge, perdeutero-4,5-ethylenedithio-1,3-dithiol-2-one is the only compound of type 1 whose mass spectrum has been described in some detail," (although some alkyland aryl-substituted 1,3-dithioI-2-ones have been studied), and (ii) we have recently reported on the differentiation and electron ionization-induced isomerization of 4,5-bis(alkylthio)-l,3-dithiole-2-thiones and their 1,2-dithioIe-3-thione isomer^.^ Thus, we reasoned that a comparative study of the mass spectra behaviour of compounds 1 and their 1,2-dithiol-3-one isomers 2 could not only reveal possible isomerizations but also show similarities and differences between the corresponding thioxo-and 0x0-analogues. Moreover, no reference to the preparation of compounds 2 has been found in the Literature, although to our surprise, an X-ray diffraction study of compound 2a has been reported.6 Thus, in this paper we report on the positiveion electron ionization (EI') mass spectra of compounds 1 and 2, along with the synthesis of compounds 2. EXPERIMENTAL ChemicalsCompounds la,' lb'" and 1c3' were prepared as previously described. Compounds 2a-c were prepared as follows. The corresponding 4,5-bis(alkylthio)-l,2-(1 mmol) was dissolved in CHCI3 (25 mL) and to this solution mercury(I1) acetate (5 mmol) and acetic acid (20mL) were added. The mixture was stirred at room temperature for 5 h and the yellow precipitate was filtered off through a celite pad and washed with dichloromethane (3 X 10 mL). The combined filtrates were washed with 1N aqueous NaHCO, and then with water. After drying (MgSO,) and evaporation of solvent under vacuum, the crude product was purified by silica column chromatography (eluent CH2CI2+hexane, 2 : l for 2a and 2c, CH2CI2 + hexane, 1 : 1 for 2b). Mass spectrometryThe mass spectra were recorded on a VG-Autospec EBE spectrometer (VG Analytical, Manchester, UK). The samples were introduced via the solids probe. The conditions for electron ionization were: electron energy 70 eV, trap current 200 PA, source temperature 200 "C. Accurate mass measurements were obtained by narrow-range voltage scanning at 10 000 resolution (measured as peak width at 5% height) using perfluorokerosene as reference compound and were correct to an accuracy of k10ppm of the theoretical value. Metastable transitions in the first field-free region were detected by linked scans'' at constant BIE and B'IE (El = E2, V = constant). Collisional experiments" were performed by colliding 8 keV ions with air in such a way that the main beam intensity was reduced to ca. 25% of its initial value. In order to ensure identical experimental conditions, the spectra of ions with the same mass value, but generated from different compounds, were recorded one after the other without adjustment of instrumental parameters. RESULTS AND DISCUSSIONThe 70eV mass spectra of compounds 1 and 2 are gathered in Table 1 and the fragmentation pattern is depicted in Scheme 1. Metastable analysis indicates that t...

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“…3170,2980,2950,2910,2860,2820,1670,1585,1490,1455,1420,1350,1310,1260,1215,1115,1070,1020,990,970,915,895,850,790,760,745, 700 cm-'. 6,33.8,28.05,27.9,25.9,25.2,25.05,24.2 (m,. -IR (KBr): 3000,2930,2860,1738,1460,1445,1370,1335,1295,1255,1230,1185,1085,1055,1003,892,802 OCH,,' J = 144 Hz),34.1,30.7,25.8,25.2,25.0,24.2 (m,.…”

Section: Experimenteller Teilmentioning

confidence: 99%

Thion‐ und Dithioester, XXX. Reaktionen von Isocyaniden mit Thiooxalestern

et al. 1982

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Tetrathiooxalsaure-dimethylester (1) bildet rnit allen untersuchten Isocyaniden 2 in einheitlicher Reaktion die 2-Imino-1,3-dithiole 4. Komplexe Produktgemische entstehen hingegen bei der Umsetzung von Dithiooxalsaure-0,O-dimethylester (5) mit Isocyaniden. Hauptprodukt ist stets das 1,3-Thiazetidin 7, Nebenprodukte sind die Azetidinthione 8 und 3,3'-Biazetidin-2,2'-dithione 6 . Thiono and Dithio Esters, XXX1) Reactions of Isocyanides with Thiooxalates

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Thion‐ und Dithioester, XXIV. Synthese von Tetrathiooxalestern

Cited by 140 publications

References 17 publications

Probing the Mott physics inκ-(BEDT-TTF)₂X salts via thermal expansion

Probing the Mott physics inκ-(BEDT-TTF)₂X salts via thermal expansion

Mass spectrometry in isomer differentiation: 4,5‐bis(alkylthio)‐1,3‐dithiol‐2‐ones and 1,2‐dithiol‐3‐ones

Thion‐ und Dithioester, XXX. Reaktionen von Isocyaniden mit Thiooxalestern

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Thion‐ und Dithioester, XXIV. Synthese von Tetrathiooxalestern

Cited by 140 publications

References 17 publications

Probing the Mott physics inκ-(BEDT-TTF)2X salts via thermal expansion

Probing the Mott physics inκ-(BEDT-TTF)2X salts via thermal expansion

Mass spectrometry in isomer differentiation: 4,5‐bis(alkylthio)‐1,3‐dithiol‐2‐ones and 1,2‐dithiol‐3‐ones

Thion‐ und Dithioester, XXX. Reaktionen von Isocyaniden mit Thiooxalestern

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Probing the Mott physics inκ-(BEDT-TTF)₂X salts via thermal expansion

Probing the Mott physics inκ-(BEDT-TTF)₂X salts via thermal expansion