hydrogenchloride; sodium hydroxide; naphthalenyllithium in ethylene glycol dimethyl ether
react. of SnBr4 with i-Pr3C6H2MgBr followed by treatment with 15percent NaOH (1st intermediate); addn. of concd. HCl (2nd intermediate); dropwise addn. of Li naphthalenide in DME at -78°C, warming to room temp. (3rd intermediate), then to 60°C; recrystn.;
参考文献
Masamune, Satoru; Sita, Lawrence R.
Journal of the American Chemical Society, 1985 , vol. 107, p. 6390 - 6391
in neat (no solvent)
slow heating of a mixt. of Ph4Sn and SnBr4 to 190°C under N2, keeping at this temp. for 2 h; dissolution of resulting oil in hexane, removing slight turbidity by filtn., cooling to -78°C, filtn., rapidly washing with cold hexane, evapn. of mother liquor yields second crop, elem. anal.;
参考文献
Schenk, Wolfdieter A.; Khadra, Almuetassem; Burschka, Christian
Journal of Organometallic Chemistry, 1994 , vol. 468, # 1-2 p. 75 - 86
Fishwick, M.; Wallbridge, M. G. H.
Journal of Organometallic Chemistry, 1970 , vol. 25, p. 69 - 79
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Gmelin Handbook: Sn: Org.Verb.1, 1.1.1.14.2, page 133 - 136
in neat (no solvent)
slow heating of a mixt. of Sn-compd. and SnBr4 to 190°C under N2, keeping at this temp. for 2 h; dissolution of resulting oil in hexane, removing slight turbidity by filtn., cooling to -78°C, filtn., rapidly washing with cold hexane, evapn. of mother liquor yields second crop, elem. anal.;
参考文献
Schenk, Wolfdieter A.; Khadra, Almuetassem; Burschka, Christian
Journal of Organometallic Chemistry, 1994 , vol. 468, # 1-2 p. 75 - 86
Foeldesi, I.
Acta Chimica Academiae Scientiarum Hungaricae, 1965 , vol. 45, p. 237 - 244
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Gmelin Handbook: Sn: Org.Verb.1, 1.1.1.8, page 113 - 114
Novikov, V. P.; Khaikin, L. S.; Vilkov, L. V.
Journal of Organometallic Chemistry, 1977 , vol. 42, p. 139 - 146
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Gmelin Handbook: F: PerFHalOrg.SVol.1, 4.4, page 66 - 70
