in neat (no solvent) byproducts: N2, ClCH2CO2CH2CH3; 1 equiv of diazoester adding slowly to an equimolar mixt. of Ge and Sn deriv. to result in exothermic reaction with N2 evolution; after 4 h at 20°C concg., diene ligand adding, heating in a sealed tube for 12h at 120°C; analyzed by gas chromy. and NMR spectroscopy;
参考文献
Castel, A.; Riviere, P.; Satge, J.
Journal of Organometallic Chemistry, 1982 , vol. 232, # 2 p. 137 - 146
acetaldehyde; triethylamine in neat (no solvent) 1 equiv of diazoester adding to a mixt. of equimolar amts. of Ge deriv.and acetaldehyde at 0°C then heating in the presence of diene ina sealed tube at 120°C; analyzed by gas chromy. and NMR spectroscopy;
参考文献
Castel, A.; Riviere, P.; Satge, J.
Journal of Organometallic Chemistry, 1982 , vol. 232, # 2 p. 137 - 146
in diethyl ether byproducts: propane, MgCl2; dry atmosphere; addn. of one equiv. of ethereal soln. of C3H7MgCl to Bu3SnH (0.125 mol); exothermic reaction; white soln. refluxed (2 h); addn. of immonium salt (0.1 mol); stirring for 2 h at room temp.; hydrolysis at 0 ° C;; extn. with ether, evapn., distn.,;
参考文献
Elissondo, Bernard; Verlhac, Jean-Baptiste; Quintard, Jean-Paul; Pereyre, Michel
Journal of Organometallic Chemistry, 1988 , vol. 339, p. 267 - 276
in diethyl ether byproducts: propane, MgClI; dry atmosphere; addn. of one equiv. of ethereal soln. of C3H7MgCl to Bu3SnH (0.125 mol); exothermic reaction; white soln. refluxed (2 h); addn. of immonium salt (0.1 mol); stirring for 2 h at room temp.; hydrolysis at 0 ° C;; extn. with ether, evapn., distn.,;
参考文献
Elissondo, Bernard; Verlhac, Jean-Baptiste; Quintard, Jean-Paul; Pereyre, Michel
Journal of Organometallic Chemistry, 1988 , vol. 339, p. 267 - 276
Sawyer, A. K.; Brown, J. E.
Journal of Organometallic Chemistry, 1966 , vol. 5, p. 438 - 445
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Gmelin Handbook: Sn: Org.Verb.4, 1.2.1.1.5.4.7, page 62 - 63
1: tri-n-butyl-tin hydride With n-butyllithium; diisopropylamine in tetrahydrofuran; hexane T=-78 - 0°C; 1 h; 2: formaldehyd in tetrahydrofuran; hexane T=-78 - 20°C; 3: With ammonium chloride in tetrahydrofuran; hexane; water
