1145663-62-2Relevant academic research and scientific papers
Synthesis of Phosphine Chalcogenides Under Solvent-Free Conditions Using a Rotary Ball Mill
Kumar, Rajnish,Kumar, Saurabh,Pandey, Madhusudan K.,Kashid, Vitthalrao S.,Radhakrishna, Latchupatula,Balakrishna, Maravanji S.
, p. 1028 - 1037 (2018)
The mechanochemical technique of ball milling has been applied to the solventless and eco-friendly synthesis of chalcogenides (sulfide and selenide) of a variety of tertiary and aminophosphines. In most of the cases, the products are obtained in almost quantitative yields with high purity by applying a simple workup procedure without using chromatographic techniques or any other purification methods. The scope of this methodology was explored by using a range of phosphines (mono, di and tetra) to synthesize partial as well as mixed chalcogenides. The use of almost equimolar amounts of starting materials and the absence of any byproducts significantly simplifies the product isolation compared with the standard solution state reactions, thus providing a highly atom economic (100 %) method with an ideal E-factor (E = 0). The solid-state reactions were monitored by 31P{1H} NMR spectroscopy. The structures of some of the products are also confirmed by single-crystal X-ray analyses. Although most of the reactions were carried out on ca. 100-mg scale, the scaling up of the reaction did not affect the course of the reaction.
Synthesis and characterizations of N,N,N′,N′-tetrakis (diphenylphosphino)ethylendiamine derivatives: Use of palladium(II) complex as pre-catalyst in Suzuki coupling and Heck reactions
Akba, Osman,Durap, Feyyaz,Aydemir, Murat,Baysal, Akin,Gümgüm, Bahattin,?zkar, Saim
experimental part, p. 731 - 736 (2009/06/19)
Oxidation of N,N,N′,N′-tetrakis(diphenylphosphino)ethylendiamine (1) with elemental sulfur and selenium gives the corresponding sulfide and selenide, respectively, [(Ph2P(E))2NCH2CH2N(P(E)Ph 2)2] (E: S 1a, Se 1b). Complexes of 1 [(M2Cl4){(Ph2P)2NCH 2CH2N(PPh2)2}] (M: Ni(II) 1c, Pd(II) 1d, Pt(II) 1e) were prepared by the reaction of 1 with NiCl2 or [MCl2(COD)] (M = Pd, Pt). The new compounds were characterized by NMR, IR spectroscopy and elemental analysis. The catalytic activity of Pd(II) complex 1d was tested in the Suzuki coupling reaction and Heck reaction. The palladium complex 1d catalyses the Heck reaction between styrene and aryl bromides as well as Suzuki coupling reaction between phenylboronic acid and arylbromides affording stilbenes and biphenyls in high yield, respectively.
