in tetrahydrofuran Heating a THF soln. of starting compds. under reflux (20 min, N2). Removal of solvent within 20 min (vac.) at a bath temp. of 70-80°C during which the green mixt. turns brown.; Removal of P4/Cr(CO)6 by sublimation (50°C, 10**-3 Torr), extn. of residue (pentane), filtn. of ext. Extg. of remaining solid (hot pentane). Crystn. of η2-P4-compd. upon slow evapn. of ext. Sepn. of product mixt. by chromy. (SiO2, hexane).;

in tetrahydrofuran Ar atmosphere, addn. of Rh complex to soln. of Cr complex and P4, stirring (room temp., 10 min), concn. to dryness (70°C, vacuum); sublimation (50°C, vacuum), suspn. (n-pentane), filtration, extn.with hot filtrate, concn. (vacuum), crystn. (5°C), sublimation ( 60°C, vacuum), crystn. (CH2Cl2, 0°C), dissolution of extd.solid (CH2Cl2), crystn. (0°C);

in tetrahydrofuran byproducts: KCl; react. of (Cr(CO)5(THF)) and PCl3 at room temp. in THF, addn. of the Mo compd. at -78°C, stirring for 1 h and slow warming to room temp.; evapn. (vac.), dissolving in benzene, filtn. (KCl), evapn., dissolving in CH2Cl2, treating with silica gel, drying (vac.), column chromy. on silica gel, elution with n-hexane-toluene and recrystn. from n-pentane;

in tetrahydrofuran byproducts: KCl; react. of (Cr(CO)5(THF)) and PCl3 at room temp. in THF, addn. of the Mo compd. at -78°C, stirring for 1 h and slow warming to room temp.; evapn. (vac.), dissolving in benzene, filtn. (KCl), evapn., dissolving in CH2Cl2, treating with silica gel, drying (vac.), column chromy. on silica gel, elution with n-hexane-toluene and recrystn. from n-pentane;

in tetrahydrofuran Irradiation (UV/VIS); (N2); 18°C, 2 h; solvent removal (vac.), sublimation (high vac.), addn. of CH2Cl2 and SiO2, partial drying, column chromy. (SiO2; hexane/toluene), recrystn. (CH2Cl2); elem. anal.;

in tetrahydrofuran; pentane addn. of Cr-compd. in THF at -40°C to soln. of phosphine in pentane, keeping for 12 h at -18°C and for 24 h at 0°C; evapn. of solvents under vac., addn. of pentane, crystn. at -78°C, elem. anal.;

in tetrahydrofuran Kinetics; byproducts: THF; 15-40°C; piperidine concn. 0.705E-2 to 30.3E-2 M; pressure 1-100 MPa; detected by UV;

in tetrahydrofuran byproducts: Cr(CO)6; Ar-atmosphere; equimolar amts.; dropwise addn. of phosphaalkyne to mixt.of metal complexes (-21°C, during 4 h), warming to 0°C; solvent removal (0.001 Torr), sublimation off of (t-BuO)3WCt-Bu and Cr(CO)6 (50°C, 0.001 Torr), dissoln. in pentane, filtration, vol. reduction (vac.), crystn.; elem. anal.;