Solak Samet, Aydemir Cemal, Karakus Mehmet, Lönnecke Peter
Department of Chemistry, Faculty of Arts & Sciences, Pamukkale University, Kinikli Denizli, 20075, Turkey.
Chem Cent J. 2013 May 20;7(1):89. doi: 10.1186/1752-153X-7-89.
The novel chiral phosphorus-1,1-dithiolates [4-CH3OC6H4P(S)(OR)S]-[H3NC(CH3)3]+ were synthesized by the reaction of [RPS2)]2 (R = 4-MeOC6H4) or P2S5 and the respective alcohol ROH (R = myrtanyl, 2-naphthylethyl, myrtenyl, borneol) in toluene. The reaction of phosphorus-1,1-dithiolates 1-4 and Au(tht)Cl, AuClPPh3 or AgNO3 and PPh3 gave rise to gold(I)- and silver(I)-complexes in THF. All compounds have been characterised by elemental analyses, IR, NMR (1H-, 13C- and 31P-) spectroscopy as well as MS measurements. Optical rotation values confirmed the chirality of the compounds. The Compound 4 has been characterized structurally by X-ray crystallography.
Phosphorus-1,1,-dithiolate compounds were formed as liquids and were treated with suitable amine in order to convert them to their salts 1-4 . They have been successfully characterized spectroscopically (IR, 1H, 13C, 31P NMR) as well as mass spectra. The compound 4 has been also structurally by X-ray crystallography. The compound 4 crystallizes in the orthorhombic space group P2(1)2(1)2(1) with Z = 4. Compounds containing phosphorus and sulfur donor atoms are excellent ligands due to offering many metal complexes especially group 11-12 metals. The synthesis of gold(I) and silver(I) complexes with chiral phosphorus-1,1,-dithiolate and triphenylphosphine have been described and investigated.
In the present work, we report the synthesis, charactreization of the chiral phosphorus-1,1-dithiolate ligands and preparing the gold(I) and silver(I) phosphorus-1,1-dithiolate or S-donor with phosphine complexes. The molecular structure of the Compound 4 was determined by X-ray diffraction. Due to an easy synthesis method of phosphorus-1,1-dithiolate compounds and a good complexion reagent, it is possible the improvement of the collecting metallic gold or silver from the minerals. When the more ionic salt of phosphorus-1,1-dithiolate compounds were prepared in this way, the water can be used as a cheap solvent. As a result, it can be an alternatively method for the collecting metallic gold or silver from the minerals in future.
新型手性磷-1,1-二硫醇盐[4-CH₃OC₆H₄P(S)(OR)S]-[H₃NC(CH₃)₃]⁺是通过[RPS₂)]₂(R = 4-MeOC₆H₄)或P₂S₅与相应的醇ROH(R = 桃金娘基、2-萘乙基、桃金娘烯基、冰片基)在甲苯中反应合成的。磷-1,1-二硫醇盐1-4与Au(tht)Cl、AuClPPh₃或AgNO₃和PPh₃在四氢呋喃中反应生成金(I)和银(I)配合物。所有化合物均通过元素分析、红外光谱、核磁共振(¹H-、¹³C-和³¹P-)光谱以及质谱测量进行了表征。旋光值证实了化合物的手性。化合物4已通过X射线晶体学进行了结构表征。
磷-1,1-二硫醇盐化合物以液体形式形成,并用合适的胺处理以将它们转化为其盐1-4。它们已通过光谱(红外光谱、¹H、¹³C、³¹P核磁共振)以及质谱成功表征。化合物4也已通过X射线晶体学进行了结构表征。化合物4在正交晶系空间群P2(1)2(1)2(1)中结晶,Z = 4。含有磷和硫供体原子的化合物由于能提供许多金属配合物,特别是第11 - 12族金属,因此是优秀的配体。已描述并研究了手性磷-1,1-二硫醇盐与三苯基膦的金(I)和银(I)配合物的合成。
在本工作中,我们报告了手性磷-1,1-二硫醇盐配体的合成、表征以及制备金(I)和银(I)的磷-1,1-二硫醇盐或含硫供体与膦的配合物。化合物4的分子结构通过X射线衍射确定。由于磷-1,1-二硫醇盐化合物的合成方法简便且是良好的络合试剂,因此有可能改进从矿物中收集金属金或银的方法。当以这种方式制备更多离子性的磷-1,1-二硫醇盐化合物时,水可作为廉价溶剂。因此,它未来可能成为从矿物中收集金属金或银的另一种方法。