copper in [3.3.1]nonane byproducts: CuS; freshly precipitated copper; Cu, sulfide and nonane heated in a sealed evacuated ampul at 160°C for 40 h; liquid decanted, solid residue washed with nonane, solns. combined, solvent removed, GLC;
参考文献
Journal of General Chemistry USSR (English Translation), , vol. 55, p. 91 - 94
Zhurnal Obshchei Khimii, , vol. 55, p. 107 - 110
acetic acid in acetic acid Kinetics; stannane was added to AcOH in a NMR tube, mixt. was kept for 20 d, reaction followed by (1)H NMR spectroscopy; ca. 29percent of the substrate was consumed, rate const. for the initial 5-10percent reaction (first 2 d) when only Me3SnOAc and Me3GeOAc were formed; not isolated, identified by (1)H NMR spectrum;
参考文献
Journal of Organometallic Chemistry, , vol. 287, p. 7 - 24
hydrogenchloride in methanol Kinetics; 8.5 M aq. HCl was added to a methanol soln. of the stannane in a NMR tube, reaction was followed by (1)H NMR spectroscopy for 50 h; 70percent of the substrate has been consumed, rate consts. according to different reaction paths are given; further products; not isolated, identified by (1)H NMR spectrum;
参考文献
Journal of Organometallic Chemistry, , vol. 287, p. 7 - 24
in tetrahydrofuran (Ar) addn. at -78°C, stirring at this temp. for 30 min, transfered to a solution of H2O in THF, warmed to -30°C for 30 min, cooling to -78°C; analyzed by gplc, mass spectrum;
in THF-d8 (tetrahydrofuran-d8) byproducts: 2,2'-bis(bromomagnesio)biphenyl, CH3MgBr; mixt. stirred in NMR tube at room temp.; after 1 h monitored by NMR; not isolated;
in tetrahydrofuran; diethyl ether; hexane byproducts: LiH; react. of TMTH with MeLi in ether/THF/hexane (2/2/1) at -125°C under Ar for 1 min; not isolated, detected by NMR;
参考文献
Reimann, Werner; Kuivila, Henry G.; Farah, Dan; Apoussidis, Theodorus
Organometallics, 1987 , vol. 6, p. 557 - 565
