hydrogenchloride in acetone
0.20 g in acetone was treated with a mixture (3 ml) of conc. HCl and an equal volume of water; stirring 15 min. at 60 °C; extraction (CH2Cl2); organic layer was separated, washed and evaporated;;
参考文献
Dhaher, Saadi M.; Eaborn, Colin; Smith, J. David
Journal of Organometallic Chemistry, 1988 , vol. 355, p. 33 - 44
in tetrachloromethane; dichloromethane
solution of ICl (1.32 mmol) in CCl4 was added dropwise (0,5 h) to a stirred solution of tin compound (1.26 mmol) in 1/4 CH2Cl2/CCl4 at room temperature; reaction was monitored by (1)H-NMR spectroscopy; solvent was removed under reduced pressure; pink residue kept under vacuum for 3 h; product was identified by comparison of its spectra with an authentic sample;
参考文献
Dhaher, Saadi M.; Eaborn, Colin; Smith, J. David
Journal of Organometallic Chemistry, 1988 , vol. 355, p. 33 - 44
in tetrahydrofuran; diethyl ether
under dry nitrogen; a THF solution of TsiLi was added with stirring (0,5 h) to a 1/3 THF/Et2O mixture of tin compound at room temperature; 1 h reflux;; solvent removed; extraction (CH2Cl2); extract was filtered and evaporated; residue was recrystd. (MeOH); elem. anal.;
参考文献
Dhaher, Saadi M.; Eaborn, Colin; Smith, J. David
Journal of Organometallic Chemistry, 1988 , vol. 355, p. 33 - 44