- Gallium and indium compounds of sulphur donor ligands: Pyridine-2-thiolates and diphenylthiophosphinates
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The reaction of GaR3 (R = tBu, Me) with 1, 2, or 3 molar equivalents of 2-mercaptopyridine (HSpy) yielded Ga(R)2(Spy) [R = tBu (1), Me(2)], Ga(R)(Spy)2 [R = tBu (3), Me (4)], and Ga(Spy)3 (5), respectively. Reaction of GaCl3 and HSpy in the presence of NEt3 does yield Ga(Spy)3 if excess HSpy is employed, otherwise Ga(Cl)(Spy)2 (NEt3) (6) may be isolated. The indium compound, In(Spy)3 (7), may be prepared both in an analogous manner to that for compound 5, but also from the reaction of HSpy with either InCl or InCl3 in the presence of NEt3. In all the compounds, except compound 3, the 2-mercaptopyridine acts exclusively as a chelating ligand. Reaction of Ga(tBu)3 with Ph2P(S)(SH) yields [Ph2P(S)S]2 but only traces of the expected product [(tBu)2Ga(μ-S2PPh2)] 2(8). In contrast, reaction of Ga(tBu)3 with HO(S)PPh2 (E = S, O) yields the dimeric compounds [(tBu)2Ga(μ-O(E)PPh2)]2, E = S (9), O (10). Compound 9 exists as a mixture of head-to-head (9a, syn) and head-to-tail (9b, anti) isomers due to the asymmetry of the bridging ligand. Reaction of GaCl3 with three molar equivalents of Na(S2PR2) ? 2(H2O), R = Me, Et, yields the tris-dithiophosphinate compounds, Ga(S2PR2) 3, R = Me (11), Et (12). All new compounds have been characterized by NMR and IR spectroscopy and mass spectrometry. In addition, the molecular structures of compounds 4 and 10 have been determined by X-ray crystallography.
- Landry, Christopher C.,Hynes, Alan,Barron, Andrew R.,Haiduc, Ionel,Silvestru, Crisian
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- Reductive Rearrangement of Tetraphenyldiphosphine Disulfide To Trigger the Bisthiophosphinylation of Alkenes and Alkynes
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The facile synthesis of organophosphorus compounds is of great importance for the development of new synthetic methods by using air-stable sources of phosphorus. In this respect, a synthetic method that is based on a reductive rearrangement and is capable of converting air-stable pentavalent phosphorus compounds into reactive trivalent phosphorus compounds is a powerful tool. Tetraphenyldiphosphine disulfide, which is a shelf-stable solid, was the focus of this study, and it was shown to undergo reductive rearrangement to trigger the bisthiophosphinylation of a variety of alkenes, such as terminal, cyclic, internal, and branched alkenes, 1,3-dienes, and terminal alkynes when exposed to light without any catalyst, base, or additive.
- Sato, Yuki,Nishimura, Misaki,Kawaguchi, Shin-ichi,Nomoto, Akihiro,Ogawa, Akiya
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p. 6797 - 6806
(2019/05/10)
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- M + 4 stable isotope labeling of levovirin and M + 7 and carbon-14 labeling of levovirin valinate pro-drug
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[M + 4]-labeled levovirin 5 (231 mg) was synthesized as an MS reference compound from [M + 4] triazole ester 2. [M + 7]-labeled levovirin valinate 6 (127 mg) was synthesized as a comparison MS reference compound from [M + 6] triazole ester 3. [14/su
- De Keczer, Steve A.,Masjedizadeh, Mohammad R.,Wu, Shao-Yong,Lara-Jaime, Teresa,Comstock, Kate,Dvorak, Charles,Liu, Yu-Ying,Berger, Walter
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p. 1223 - 1236
(2007/10/03)
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- A Convenient Preparation of Bis(phosphorothioyl) Sulfides
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The reaction of piperidinium and potassium phosphorodithioates with 2-chloro-1-methyl-pyridinium salts afforded the corresponding bis(phosphorothioyl) sulfides in good yields.The similar reaction with potassium diphenylphosphorothioate gave exclusively bis(diphenylphosphorothioyl) oxide. - Keywords: Bis(phosphorothioyl) Sulfides, Piperidinium Phosphorodithioates, Bis(phosphorothioyl) Oxides
- Min, Shi,Ishihara, Hideharu,Murai, Toshiaki,Kato, Shinzi
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p. 153 - 157
(2007/10/02)
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- REACTIONS OF DIALKYL DITHIOPHOSPHORIC AND DIPHENYLDITHIOPHOSPHORIC ACIDS WITH THIOCYANATES
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The interaction between phosphorus(IV) dithio acid partial esters and thiocyanates proceeds with initial formation of addition products to the CN bond.These adducts are either split by the second molecule of dithio acid to S-alkyl dithiocarbamates and tetraalkyl trithiophosphates or rearrange into dialkyl N-thiophosphoryldithiocarbamates.The latter easily split off the thiols and convert to isothiocyanatothiophosphates.A number of thiophosphorylated and diphosphorylated thioureas were synthesized by the reaction of isothiocyanatothiophosphates with amines and α-aminoalkylphosphonates.
- Zimin, M. G.,Kamalov, R. M.,Cherkasov, R. A.,Pudovik, A. N.
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p. 371 - 378
(2007/10/02)
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