The reaction of phosphine dichlorides with 1- or 2-alkanethiols or benzenethiol in the presence of triethylamine and subsequent distillation afforded phosphines and disulfides in good yields. The reaction was shown to be useful for reduction of tertiary phosphine oxides to the corresponding phosphines.
The crystal and molecular structures of dichlorobis(2-pyridinethiolato)tin(IV) have been determined by X-ray analysis. The crystal belongs to the triclinic system: a=8.340(8), b=12.456(7), c=7.178(3) Å, α=86.46(4), β=111.06(5), γ=99.18(6)°, space group P\bar1 with Z=2. The structure was determined by the heavy atom method and refined by the block-diagonal least-squares method (R=0.058). The complex is a distorted octahedral complex in which 2-pyridinethiolato ligands act as bidentate ligands, two four-membered (Sn, S, C, and N) chelate rings being present. Two Sn–Cl bonds are cis, two Sn–N bonds are cis, and two Sn–S bonds are trans configuration.
In the presence of a tertiary amine, sodium borohydride (NaBH4) combined with zinc chloride (ZnCl2) showed powerful reducing properties and carboxylic esters were smoothly reduced to their corresponding alcohols which were not obtained by reduction with NaBH4 and ZnCl2 alone. Tetrahydrofuran (THF) was an efficient solvent, and the effective molar ratio of the reducing agents, NaBH4 : ZnCl2 : tertiary amine, was 2 : 1 : 1. In particular, aminobenzoates such as anthranilic esters, were reduced to aminobenzyl alcohols with high yields without the addition of a tertiary amine. Further, it was also found that this combination reduced nitro, cyano, and amido groups to their corresponding amino groups.
scite is a Brooklyn-based organization that helps researchers better discover and understand research articles through Smart Citations–citations that display the context of the citation and describe whether the article provides supporting or contrasting evidence. scite is used by students and researchers from around the world and is funded in part by the National Science Foundation and the National Institute on Drug Abuse of the National Institutes of Health.