n-butyllithium; diisopropylamine in tetrahydrofuran; hexane T=-50°C; 1 h;
参考文献
Hulst, Ron; Muizebelt, Inouk; Oosting, Peter; Van Der Pol, Cornelia; Wagenaar, Anno; Smisterova, Jarmila; Bulten, Erna; Driessen, Cecile; Hoekstra, Dick; Engberts, Jan B. F. N.
European Journal of Organic Chemistry, 2004 , # 4 p. 835 - 849
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: 1.0 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.; (119Sn NMR monitoring);
参考文献
Marton, Daniele; Tari, Massimo
Journal of Organometallic Chemistry, 2000 , vol. 612, # 1-2 p. 78 - 84
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: 3.5 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
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: 5.5 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
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: 3.5 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
