zinc in tetrahydrofuran; water under air atm., at room temp., cosolvent media: H2O(NH4Cl)/THF/Zn, alkyliodide was added dropwise to the alkyl tin halide in solvent mixt. over 15 min, reaction time: 1.5 h; Zn was filtered off, aq. phase was extd. three times with n-pentane, organic phase was washed with sat. aq. NaCl and dried over MgSO4, solvent was removed, crude oil was distilled under vac., then chromd. using n-hexane; (119Sn NMR monitoring);
参考文献
Marton, Daniele; Tari, Massimo
Journal of Organometallic Chemistry, 2000 , vol. 612, # 1-2 p. 78 - 84
in ethanol byproducts: NaCl; mixing, refluxing for 1 h; cooled, solvent removed in vac., residue heated in hexane/CHCl3 (10:1), filtered, crystn. (on cooling);
参考文献
Deeth, Robert J.; Molloy, Kieran C.; Mahon, Mary F.; Whittaker, Sophie
Journal of Organometallic Chemistry, 1992 , vol. 430, # 1 p. 25 - 35
n-butyllithium in tetrahydrofuran (protected from light and O2); BuLi/THF added at-78°C under N2 to2-bromo-5-dioxolanylthiophene/THF, stirred for 1 h at -78°C, Sn compd. added, reacted for 1 h 30 min; H2O and Et2O added, the org. layer extd. (H2O and satd. soln. of NH4Cl),the org. phase dried (MgSO4), evapd. (vac.), distd.;
参考文献
Prim, Damien; Auffrant, Audrey; Plyta, Zoi F.; Tranchier, Jean-Philippe; Rose-Munch, Francoise; Rose, Eric
Journal of Organometallic Chemistry, 2001 , vol. 624, # 1-2 p. 124 - 130
