in neat (no solvent) 2,2-bis(trimethylstannyl)propane placed in flash with 2 mol of dimethyldichlorostannane, heated at 60°C overnight; stirred at 15-20 Torr, warmed at 0.01 Torr to 100°C, recrystd. (CCl4); elem. anal.;
in dichloromethane Kinetics; (MCOT)PtCl2 is dissolved in CH2Cl2, (CH3)3Sn(ClC6H4) is added by syringe, soln. is stirred for 10 min.; Ppt. filtered off, washed with CH2Cl2, dried in air, elem. anal., ratio trans:cis=3:1.;
phosphorus trichoride in tetrahydrofuran exclusion of air, moisture; (Ar); soln. of PCl3 in THF was dropped to soln. of (t-Bu)2PSnMe3 in THF under stirring within 30 min at -10°C (molar ratio 3:1); yellow soln. was heated to room temp.; primary yield ca. 60 P-percent; ((31)P NMR); removal of solvent at -30°C under vac.; dissolved residue in cold n-pentane; soln. was stored for 12 h at -30°C (separated Me3SnCl); removal of solvent at -30°C; purifn. of prod. with HPLC;;
参考文献
Zeitschrift fuer Naturforschung, Teil B: Chemical Sciences, , vol. 44, p. 375 - 380
in diethyl ether addn. of P-compound in soln. to stirred soln. of stannane at -50-70°C; solvent removed, (CH3)3SnCl isolated, extn. with ether (5 times), solvent removed; elem. anal.;
参考文献
Journal of General Chemistry USSR (English Translation), , vol. 57, p. 47 - 51
Zhurnal Obshchei Khimii, , vol. 57, p. 56 - 63
