methanol in pentane N2 atmosphere; addn. of MeOH to B-compd. in pentane (-78°C), stirring (1 h); removal of solvent (vac.), distn. (64°C, 20 Torr and 80-82°C, 0.1 Torr);
参考文献
Frankhauser, Pascal; Driess, Matthias; Pritzkow, Hans; Siebert, Walter
Chemische Berichte, 1992 , vol. 125, # 6 p. 1341 - 1350
in tetrahydrofuran under Ar, stirred for 3 h at 20°C; removal of the volatiles, recrystn. from toluene at -78°C, dried in vac. (20°C, 1 h); detn. of intermediates by NMR-spectroscopy;
参考文献
Schaefer, H.; Binder, D.
Zeitschrift fuer Anorganische und Allgemeine Chemie, 1988 , vol. 557, p. 45 - 58
in tetrahydrofuran under Ar, stirred for 2 h at 20°C; volume reduced, cooled to -78°C for 2 d, pptn. of (DPPE)2Ni, evapn. of mother liquor, recrystn. from toluene at -20°C, dried in vac. (20°C, 1 h); elem. anal.;
参考文献
Schaefer, H.; Binder, D.
Zeitschrift fuer Anorganische und Allgemeine Chemie, 1988 , vol. 557, p. 45 - 58
in tetrahydrofuran under Ar, THF soln. of (DCPE)NiCl2 frozen by liquid N2, addn. of (CH3)3SiPH2, mixt. warmed to -20°C and stirred for 12 h; volume reduced in vac. at -20°C, cooled for 24 h at -78°C, pptn., filtration at -20°C, dried in vac. at -20°C;
参考文献
Schaefer, H.; Binder, D.
Zeitschrift fuer Anorganische und Allgemeine Chemie, 1988 , vol. 557, p. 45 - 58