however, this reaction requires an inert atmosphere. While W(CO)6 reacts rapidly with amines to give cis diamine adducts in high yields, direct reactions with phosphines are not so clean. Bis(phosphine) complexes are, however, cleanly formed when a small amount of piperidine is added to the reaction mixture, presumably via the bis(piperidine) complex cis-[W(CO)4(pip)2]. Reactions with Cr(CO)6 generally
Sonochemistry and sonocatalysis of metal carbonyls
作者:Kenneth S. Suslick、James W. Goodale、Paul F. Schubert、Hau H. Wang
DOI:10.1021/ja00356a014
日期:1983.9
67 The labeled precursor utilized in the present investigation, 1-deoxy-D-three [ l-2H3,5-2Hl]pentulose (6) was synthesized from 2,4-O-benzylidene-~-[4-~H~] threose, which is available from D[ l-2Hl]arabinitol by standard Reaction of the threose derivative with trideuteriomethylmagnesium iodide in ether then gave a mixture of protected, epimeric pentane tetrols, which was oxidized by the stannylene
然后提取硫胺素,并用亚硫酸氢盐裂解,以通常的方式得到 HET。将其转化为三氟乙酸酯用于 MS 检查。
Crystal structures of [W(CO)5(PPh3)], [M(CO)5(AsPh3)] and [M(CO)5(SbPh3)](M = Mo or W): a comparative study of structure and bonding in [M(CO)5(EPh3)] complexes (E = P, as or Sb; M = Cr, Mo or W)
作者:Manuel J. Aroney、Irmi E. Buys、Murray S. Davies、Trevor W. Hambley
DOI:10.1039/dt9940002827
日期:——
Crystal structures have been determined for [W(CO)5(PPh3)], [M(CO)5(AsPh3)] and [M(CO)5-(SbPh3)](M = Mo or W) as part of a systematic study of a series of nine [M(CO)5(EPh3)] complexes (M = Cr, Mo or W; E = P, As or Sb). Trends in bond lengths and angles are rationalised in terms of steric and electronic interactions between the bonded M(CO)5 and EPh3 fragments. Comparison is made between the solid-state
Exploring the coordination chemistry and reactivity of dialkylamino- and bis(dialkylamino)-phosphines in the coordination sphere of metals
作者:Philip W. Dyer、John Fawcett、Martin J. Hanton、Raymond D. W. Kemmitt、Ranbir Padda、Narendra Singh
DOI:10.1039/b208886j
日期:2003.12.20
[RhCl(CO)2}2] and elemental selenium have been undertaken and the products used to assess the phosphines' donor capabilities. Depending on the substituents at phosphorus, either trans-diphosphine or cis-dicarbonyl complexes result from reaction with [RhCl(CO)2}2]. The sterically demanding phosphine P(NPri2)2Ph (5) proved unreactive towards complexation with metals, although its selenide could be prepared and
一系列二烷基氨基和双(二烷基氨基)的配位化学-phosphines,R X P(NR' 2)3 - X (X = 1或2; R =氯,甲基中,Ph,C 6 ˚F 5 ; R' = Et,Pr i),1–7,已进行了研究,所得的6族四羰基和二氯化铂双(膦)复杂的特征。随后,与金属结合的PN键的反应性膦类被探测了。R“ OH(R” = Me,Et,烯丙基)双(dialkylaminodiphenylphosphine)与导致NR'的取代无水HCl气体络合物溶液2由OR“; 分离得到的P-烷氧基配合物,收率极高。酸化乙二醇 解决方案 氨基膦配合物得到相应的双(氯二苯基膦)衍生物。以下的反应的反式- [W(CO)4(P 净2 }博士2)2与]任HCl水溶液或H 2 SO 4,反式- [W(CO)4(P OH}博士2)2 ]可以被隔离为二氯甲烷溶剂化物,收率极高(81%)。双(双(二二烷基氨基
The application of microwave dielectric heating to the synthesis of arene-metal complexes. Synthesis of [(η-arene)(CO)3Mn]PF6 complexes and [(η-arene)(η-cyclopentadienyl)Fe][PF6] complexes with triphenylphosphine, tert-butylbenzenes and a sterically hindered phenol as arene ligands
作者:Q. Dabirmanesh、R.M.G. Roberts
DOI:10.1016/s0022-328x(97)00289-1
日期:1997.9
Microwave-mediated synthesis of [(η-arene)(CO)3Mn](PF6) complexes are reported. Reaction times are reduced from several hours by conventional methods to a few minutes using an unmodified domestic microwave oven. The synthesis of a bis complexed triphenylphosphine iron sandwich complex, [((η-C6H5)(η-Cp)Fe]2 PC6H5][PF6]2 is reported from AlCl3-catalysed ligand exchange reactions between ferrocene and
报道了微波介导的[(η-芳烃)(CO)3 Mn](PF 6)配合物的合成。使用未经改造的家用微波炉,反应时间从常规方法的几小时减少到几分钟。由AlCl 3催化之间的配位体交换反应报道了双配合物三苯基膦铁夹心配合物[[((η- C6 H 5)(η-Cp)Fe] 2 PC 6 H 5 ] [PF 6 ] 2的合成。二茂铁和M(CO)4(PPh 3)2配合物(MCr,Mo,W)。立体受阻[[η-arene)(η-Cp)Fe] [PF 6使用上述微波技术已经以中等至优异的产率制备了具有叔丁基取代基的]配合物。试图合成甲基环戊二烯基类似物导致明显的脱烷基。在后一种配合物中没有发现限制旋转的证据。报道了直接合成1,3,5-三甲基苯酚铁夹心复合物。这是通过铁夹心化学中的配体交换反应制备的苯酚配合物的第一个例子。