sodium hydroxide; water; dihydrogen peroxide in tetrahydrofuran; water
to soln. of Sn compd. in THF added soln. of BH3 (B/Sn ratio 1/1) in THF under N2 at room temp., stirred 1 h, refluxed 1h, cooled to room temp., added H2O, added soln. of 3 M NaOH in 30percent H2O2, stirred for 30 min; added Et2O, extd. (3 M NaOH), acidified with dil. HCl, extd. (Et2O);
参考文献
Pickles, G. M.; Spencer, T.; Thorpe, F. G.; Chopa, A. B.; Podesta, J. C.
Journal of Organometallic Chemistry, 1984 , vol. 260, # 1 p. 7 - 16
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
Adams, Harry; Bailey, Neil A.; Bentley, Gary W.; Hough, Gordon; Winter, Mark J.; Woodward, Simon
Journal of the Chemical Society, Dalton Transactions: Inorganic Chemistry (1972-1999), 1991 , # 4 p. 749 - 758