- Efficient one-pot synthesis of secondary cyclic phosphanes with easy regeneration of the phosphorus-donor reagent used
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Phosphanes: No pain, all gain. A regenerable phosphorus donor is the key to an efficient and economic one-pot synthesis of five- and six-membered secondary cyclic phosphanes. The reaction, at room temperature, of 1 with 1 equivalent of bis(Grignard reagent) 2 followed by treatment with aqueous acid gives cyclic phosphanes 3 in 70-80% yield and the new compound 4. Simply treating 4 with PCl3 quantitatively regenerates the starting reagent 1, which can be reused without further purification.
- Baccolini, Graziano,Boga, Carla,Galeotti, Matteo
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- Oligodentate Phosphine Ligands with Phospholane End Groups: New Synthetic Access and Application to Molybdenum-Based Synthetic Nitrogen Fixation
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A new synthetic access to oligodentate phosphine ligands with phospholane end groups, starting from lithium phospholanide, is established. Based on this building block, the tridentate ligand prPP(Ph)P-pln was synthesized and used for the synthesis of [MoX3{prPP(Ph)P-pln}] (X = Cl, Br, I) precursors. Sodium amalgam reduction in the presence of N2 and either mono- or bidentate ligands leads to several molybdenum(0) mono- and bis(dinitrogen) complexes, respectively. With the diphosphine dppm a mixture of facial and meridional isomers of [Mo(N2){prPP(Ph)P-pln}(dppm)] is formed. Using the monophosphines PMePh2 and PMe2Ph mer-[Mo(N2){prPP(Ph)P-pln}(PMe2Ph)2] and trans-[Mo(N2)2{prPP(Ph)P-pln}(PMePh2)] could be obtained. The spectroscopic properties and reactivity of the latter towards protonation was investigated, and a hydrazido complex could be obtained and characterized.
- Pfeil, Mareike,Engesser, Tobias A.,Koch, Alexander,Junge, Jannik,Krahmer, Jan,N?ther, Christian,Tuczek, Felix
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p. 1437 - 1448
(2019/12/24)
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- Flash vacuum pyrolysis of dichlorophosphines over magnesium: Generation and reactivity of simple phosphinidenes
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Flash vacuum pyrolysis of dichlorophosphines over magnesium at 500-600 °C gives the products expected from intramolecular CH insertion of the corresponding phosphinidenes.
- Aitken, R. Alan,Masamba, Wayiza,Wilson, Neil J.
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p. 8417 - 8420
(2007/10/03)
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- Process for preparing cyclic phosphinic acid esters
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Process for preparing cyclic phosphinic acid esters of the formula (I) STR1 wherein R1 is an alkyl radical having up to 18 carbon atoms or a phenyl radical being optionally substituted by alkyl, halogen or alkylated amino groups, R2 stands for a hydrogen atom or has the same meaning as R1 and n is 1 or 2, which comprises reacting phosphinic acid monoesters of the formula (II) STR2 wherein R3 is an alkyl radical having up to 8 carbon atoms optionally substituted by chlorine atoms and R1 has the meaning given above, with an alkenol of the formula (III) STR3 wherein R2 and n have the aforesaid meaning, in the presence of catalytic quantities of free radical forming agents, splitting off the alcohol of formula (IV) simultaneously or subsequently and separating the reaction products, preferably by distillation.
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