15573-38-3Relevant articles and documents
Role of acid in precursor conversion during InP quantum dot synthesis
Gary, Dylan C.,Cossairt, Brandi M.
, p. 2463 - 2469 (2013)
We have studied the speciation of P(SiMe3)3 during the synthesis of colloidal InP quantum dots in the presence of proton sources. Using 31P NMR spectroscopy, we show H3-nP(SiMe 3)n formation on exposure of P(SiMe3) 3 to a variety of protic reagents including water, methanol, and carboxylic acid, corroborating observations of P(SiMe3)3 speciation during the hot injection synthesis of InP QDs. Quantitative UV-vis comparisons between InP growth from P(SiMe3)3 and HP(SiMe3)2 show unambiguously that when total H +-content is accounted for, particle size, size dispersity, and concentration are indistinguishable for these two reagents. The dual role of myristic acid in P-Si bond cleavage and as a source of the myristate anion, an essential component of the quantum dot surface, is interrogated using tetrabutylammonium myristate, confirming that it is the protons that are responsible for increased quantum dot polydispersity. Together these data support the existence of a competing acid-catalyzed pathway in the conversion of P(SiMe3)3 to InP and demonstrate its impact. By preventing a constant solute supply and affecting the concentration of quantum dot surfactant over the course of the reaction, the existence of competing precursor conversion pathways is detrimental to formation of monodisperse colloids, explaining much of the irreproducibility in InP quantum dot syntheses to date.
A Simple Method for the Preparation of Tris(trimethylsilyl)phosphine
Niecke, E.,Westermann, H.
, p. 330 (1988)
Tris(trimethylsilyl)phosphine is prepared in good yield by the reation of piperidinodichlorophosphine with lithium and chlorotrimethylsilane in boiling tetrahydrofuran.
Synthesis and X-ray crystal structure of novel tetramethylphosphonium dichlorodimethylaluminate
Bani-Fwaz, Mutasem Z.
, p. 956 - 963 (2020)
The reaction of tris(trimethylsilyl)phosphine with dimethylaluminum chloride in 1,2-dimethoxyethane (monoglyme) displays an important role as building blocks that results in the production of novel tetramethyl phosphonium dichlorodimethylaluminate and the already known dimer compound (bis(2,2-methoxy-ethanolato-O,O′)-tetramethyl-di-aluminum). The newly formed tetramethyl phosphonium dichlorodimethylaluminate [(CH3)4P]+[(CH3)2AlCl2]? crystallizes in the monoclinic space group P21/c, having unit cell with lattice constants a = 7.522, b = 11.644, c = 14.841 ?, and β = 99.32° includes four formula units. The mean values of the bond lengths are P-C 1.787 ?, Al-Cl 2.224 ?, and Al-C 1.966 ?. Both phosphorus and aluminum are tetrahedrally surrounded in organophosphonium-based cations and organoaluminium-based anions. The geometry of the dichlorodimethylaluminate anion shows a distorted tetrahedron.
Fritz et al.
, p. 266,269 (1974)
1-Heteroakylation of tris(trimethylsilyl)phosphine
Prishchenko, Andrey A.,Livantsov, Mikhail V.,Novikova, Olga P.,Livantsova, Ludmila I.,Petrosyan, Valery S.
, p. 441 - 445 (2010)
The 1-heteroalkylation of the tris-(trimethylsilyl)phosphine was thoroughly investigated using heterosubstituted methylamines, chloromethyl alkyl ethers, methyl chloroformate, paraformaldehyde, and dialkylformamides. Convenient methods for the synthesis of tris(dialkylaminomethyl)phosphines, tris(alkoxymethyl)phosphines, tris(methoxycarbonyl) phosphine, and several phosphaethylenes were proposed on the basis of the 1-heteroalkylation of tris(trimethylsilyl)phosphine as a valuable synthon.
Simple conversion of trisodium phosphide, Na3P, into silyl- and cyanophosphides and the structure of a terminal silver phosphide
Grützmacher, Hansj?rg,Le Corre, Grégoire
supporting information, p. 3497 - 3501 (2022/03/14)
A reaction of trisodium phosphide (Na3P) with chlorosilanes allows for simple derivatization into silyl- and cyano-substituted phosphanide species which were compared with each other. The recently discovered cyano(triphenylsilyl)phosphanide shows unique coordination properties compared to bis(silyl)phosphides.
Exploration of Novel α,ω-Substituted Diphosphatrisilanes by Combining Experimental Methods and DFT Calculations
Weinberger, Gernot P.,Sommer, Florian,Torvisco, Ana,Fischer, Roland C.,Flock, Michaela
, p. 3778 - 3785 (2020/09/09)
The novel diphosphatrisilanes {(R2P-Si(SiMe3)2-)2-SiMe2} [R = Ph, H] and the cyclophosphatrisilabutanes {R–PSi3} [R = H, SiMe3] have been prepared via salt metathesis reactions between phosphanides and 2,4-dihalogenated pentasilanes and characterized via NMR spectroscopy. The experimental results were supported by DFT calculations. Although P–Si bond formation was observed in all cases, the outcome of the reactions varied depending on the nature of ligands on the phosphanides, forming either linear diphosphatrisilanes or cyclic phosphatrisilacyclobutanes. DFT studies were performed to get a better understanding of the reactions. The precursor silanes were fully characterized using NMR spectroscopy and single-crystal X-ray diffraction and offer interesting building blocks. In addition, a modified route for the synthesis of P(TMS)3 was successfully carried out, achieving high yields of up to 73 %, circumventing the use of white phosphorus and phosphine gas during the reaction.
