phosphorus trichoride in tetrahydrofuran T=-78 - 20°C; 16 h;

phosphorus trichoride

triethylamine

in toluene exclusion of moisture, Schlenk technique; soln. of B-compound in toluene refluxed (48 h); distn. (90°C/1E-2 Torr), mixt. of both products, detected by NMR;

in neat (no solvent) exclusion of moisture, Schlenk technique; B-compound heated (4 h, 180°C); distn. (48°C/1E-2 Torr), mixt. of both products, detected by NMR;

(i) nBuLi, Et2O, hexane, (ii) PCl3; Multistep reaction;

in dichloromethane dropwise addn. of (ClPN((CH3)3C))2 in CH2Cl2 to soln. of ((CH3)2SnN((CH3)3C))2 in CH2Cl2 under stirring; refluxing for 3 h; filtration; performed under N2;; evapn.; sublimation at 50°C and 2E-6 Torr for 2 d with isolation of (CH3)2SnCl2; dissolving residue in CH2Cl2 and repeated sublimation; dissolving residue in CH2Cl2 and cooling to -20°C with isolation of stannabicycloheptane; elem. anal.;;

in chloroform under Ar, nickel complex and CHCl3 soln. of ligand (molar ratio 1:2) stirred at 0°C for 1 h; filtered, filtrate mixed with ether, decanted, washed with ether until solidification, dried in vac., elem. anal.;

in chloroform under Ar, nickel complex and CHCl3 soln. of ligand (molar ratio 1:1) mixed at -30°C, stirred for 10 min; filtered, dropped to cooled ether, filtered, dried in vac., elem. anal.;

in tetrahydrofuran byproducts: NaCl; Mn-complex and ligand in THF were stirred for 10 h at -78°C, mixt. was warmed to 25°C and refluxed for 10 h;; filtered, Mn2(CO)10 evapd. in vac., redissolved in THF, crystals were obtained at 0°C from soln.;;