in neat (no solvent) inert atmosphere; slow addn. of dichlorostibine to eexcess of Bu3SnH (room temp.) with continuous fractional distn. of product (vac., condensing at -196°C);
in further solvent(s) byproducts: 1-butene; addn. of stannane to soln. of BCl3 (1.3 equiv. in 1,1,2,2-tetrachloroethane) at -40°C, stirring for 10 min at -40°C; trap-to-trap distn. (removing solvent at -50°C, distn. of productat -80°C); NMR spectroscopy (isomers not sepd., Z:E ratio 1:1);
参考文献
Le Serre, Stephanie; Guillemin, Jean-Claude
Organometallics, 1997 , vol. 16, # 26 p. 5844 - 5848
in further solvent(s) addn. of stannane to soln. of BCl3 (1.3 equiv. in 1,1,2,2-tetrachloroethane) at -40°C, stirring for 10 min at -40°C; trap-to-trap distn. (removing solvent at -50°C, distn. of productat -80°C); NMR spectroscopy;
参考文献
Le Serre, Stephanie; Guillemin, Jean-Claude
Organometallics, 1997 , vol. 16, # 26 p. 5844 - 5848
in neat (no solvent) High Pressure; (Ar); addn. of GeCl4 to tin compd., heating to 150°C for 12 h in a sealed tube, cooling to room temp.; dissolving in CH2Cl2, vac. distn.;
参考文献
Kultyshev, Roman G.; Prakash, G.K. Surya; Olah, George A.; Faller, Jack W.; Parr, Jonathan
Organometallics, 2004 , vol. 23, # 13 p. 3184 - 3188
Delmond, B.; Pommier, J. C.; Valade, J.
Comptes Rendus des Seances de l'Academie des Sciences, Serie C: Sciences Chimiques, 1972 , vol. 275, p. 1037 - 1040
in chloroform-d1; dichloromethane-d2 in CDCl3/CD2Cl2 = 1:1 at 0.5 M at -90°C (allyl)Bu3Sn was instantaneously consumed and only (allyl)2SnCl2 and Bu3SnCl were detected within 5 min.; NMR;
参考文献
Journal of the American Chemical Society, , vol. 110, p. 984
