in tetrahydrofuran; diethyl ether; ammonia byproducts: CaCl2; NH3 (liquid); (N2); charging of Ca in dry box Schlenk tubes with (SnPh3)2; addn. of THF, cooling to -78°C; condensation of pre-dried liq. NH3 onto react. mixt., reflux for 6 h at -33°C; warming to room temp.; evapn. of NH3, addn. of 1N HCl soln. in Et2O; removal of volatiles in vac., dissolving in Et2O, filtration through Celite padded filter frit, removal of solvent;
参考文献
Journal of Organometallic Chemistry, , vol. 613, # 2 p. 139 - 147
in tetrahydrofuran; diethyl ether; ammonia byproducts: SrCl2; NH3 (liquid); (N2); charging of Sr in dry box Schlenk tubes with (SnPh3)2; addn. of THF, cooling to -78°C; condensation of pre-dried liq. NH3 onto react. mixt., reflux for 6 h at -33°C; warming to room temp.; evapn. of NH3, addn. of 1N HCl soln. in Et2O; removal of volatiles in vac., dissolving in Et2O, filtration through Celite padded filter frit, removal of solvent;
参考文献
Journal of Organometallic Chemistry, , vol. 613, # 2 p. 139 - 147
in tetrahydrofuran Ar atmosphere, RYbI transferring dropwise under Ar pressure at room temperature, 2 to 3 h, Me3SnCl addn.; extracting with ether, extracts drying (Na2SO4);
参考文献
Russian Journal of General Chemistry, , vol. 67, # 1 p. 76 - 78
in tetrahydrofuran under Ar; addn. of freshly prepd. THF soln. of PhSmI to mixt. of THF and Ph3SnSnPh3, mixing at 25°C for 3 h, decompn. of react. mixt. with water acidified with HCl; thin layer chromy.;
参考文献
Russian Journal of General Chemistry, , vol. 70, # 2 p. 244 - 246
Zasosov, V. A.; Kocheshkov, K. A.
Sb. Statei Obshch. Khim. Akad. Nauk SSSR, 1953 , vol. 1, p. 285 - 289
Full Text Show Details
Gmelin Handbook: Sn: Org.Verb.1, 1.1.1.16.1.1, page 141 - 147
Zasosov, V. A.; Kocheshkov, K. A.
Sb. Statei Obshch. Khim. Akad. Nauk SSSR, 1953 , vol. 1, p. 285 - 289
Full Text Show Details
Gmelin Handbook: Sn: Org.Verb.1, 1.1.1.16.1.1, page 141 - 147
in benzene byproducts: perfluorocyclopropane; absence of air and moisture; heating of Sn-compd. 2 equiv. of Hg-compd. (sealed tube, 125°C, 3 weeks); not isolated, detd. by (19)F-NMR spectroscopy;
参考文献
Eujen, Reint; Lagow, Richard J.
Journal of the Chemical Society, Dalton Transactions: Inorganic Chemistry (1972-1999), 1978 , p. 541 - 544
