title: Reactivity of Elemental Tin and Zinc toward Organophosphonic Acid Dialkyl Esters: A New One-Pot Recipe for the Synthesis of Coordination Assemblies Derived from O-Alkylorganophosphonate Ligands.
abstract: A new recipe for the synthesis of diorganotin bis(O-alkylorganophosphonate)s, R12Sn{O(P)(O)(OR1)R}2[R = R1= methyl (1); R1= ethyl and R = methyl (2), allyl (3), 2-thienyl (4), benzyl (5)], has been developed from the direct reaction of elemental tin (powder) with organophosphonic acid dialkyl esters, RP(O)(OR1)2, in the presence of a catalytic amount of potassium iodide under ambient conditions (130 °C, 18-20 h). The key steps in the proposed catalytic cycle involve the monodealkylation of phosphonate diester and in situ generation of a R1SnI or R12SnI2intermediate via the oxidative addition of alkyl iodide on tin. Evidence in support of the formation of organotin species comes from the isolation of Me2Sn{O(P)(O)(OiPr)Me}2(6) from the direct reaction of tin metal with MeP(O)(OiPr)2in the presence of methyl iodide. The method has also been extended to isolate Zn{OP(O)(OMe)Me}2(7) using metallic zinc as the precursor. All of the compounds have been characterized by IR and NMR studies as well as X-ray crystallography for 2, 4, 6, and 7.
authors.affiliation: Department of Chemistry, Indian Institute of Technology , Hauz Khas, New Delhi 110016, India.
authors.forename: Ravi
authors.identifier: http://orcid.org/0000-0002-4991-7018
authors.initials: R
authors.lastname: Shankar
authors.affiliation: Department of Chemistry, Indian Institute of Technology , Hauz Khas, New Delhi 110016, India.
authors.forename: Swati
authors.initials: S
authors.lastname: Mendiratta
authors.affiliation: Department of Chemistry, Indian Institute of Technology , Hauz Khas, New Delhi 110016, India.
authors.forename: Nisha
authors.initials: N
authors.lastname: Singla
authors.affiliation: Department of Chemistry, University of Bath , Bath BA2 7AY, U.K.
authors.forename: Gabriele
authors.initials: G
authors.lastname: Kociok-Köhn
authors.affiliation: Lehrstuhl für Anorganische Chemie II, Technische Universität , 44221 Dortmund, Germany.
authors.forename: Michael
authors.initials: M
authors.lastname: Lutter
authors.affiliation: Lehrstuhl für Anorganische Chemie II, Technische Universität , 44221 Dortmund, Germany.
authors.forename: Klaus
authors.initials: K
authors.lastname: Jurkschat