Preparations of metal trichalcogenophosphonates from organophosphonate esters
A new method for the preparation of metal trichalcogenophosphonates is presented wherein organophosphonate esters are first reduced with LiAlH 4 and subsequently treated with an organometallic reagent and elemental sulfur or selenium to give th
Davies, Robert P.,Patel, Laura,White, Andrew J. P.
p. 11594 - 11601,8
(2020/10/15)
Preparation of primary and secondary alkyl phosphines from elemental phosphorus or phosphorus trichloride in organic solvents
A number of volatile and non-volatile primary and secondary alkyl phosphines have been prepared by one-pot procedures from elemental phosphorus or from phosphorus trichloride. The element or chloride was first converted into trisodium phosphide by reaction with sodium in the presence of naphthalene or another solubilisation reagent. Subsequent addition of two equivalents of t-butyl alcohol and an alkyl halide gave monoalkyl phosphines in fair to good yields. In situ conversion of the primary phosphine into a dialkyl phosphine was achieved by metallation with BuLi or sodium and subsequent alkylation.
Van Hooijdonk,Gerritsen,Brandsma
p. 39 - 49
(2007/10/03)
SYNTHESIS OF PRIMARY α-CHLOROPHOSPHINES BY A CHEMOSELECTIVE REDUCTION OF α-CHLOROPHOPHONATES
Reduction of chloromethylphosphonates with lithium aluminium hydride gave a mixture of chloromethylphosphine and methylphosphine, characterized by NMR, IR and mass spectra.Reduction of the same compounds by AlH3 gave chloromethylphosphine as nearly the only product.Extension of this reaction to the C-substituted derivatives gave the correspondeng α-chlorophosphines with good chemoselectivity.Keywords: Reduction of phosphonates; aluminium hydride; chemoselectivity; primary phosphines.