in 1,4-dioxane T=0 - 20°C;

in tetrahydrofuran; toluene byproducts: HP(C(CH3)3)2, P2(C(CH3)3)4; LiP(C(CH3)3)2 suspended in toluene, cooled to -78 °C, GaBr soln. in 3:1 toluene/THF added dropwise, mixt. stirred, warmed to room temp. over 6 h, soln. heated to 50 °C for 1 h under reduced pressure; soln. filtered, solvent removed (vac.), residue redissolved (toluene), filtered, toluene extract stored at 7 °C for crystallization for several weeks;

1: 40 percent / tetrahydrofuran / 24 h / 20 °C 2: Ambient temperature View Scheme

in tetrahydrofuran byproducts: LiCl; all manipulations under dry, O2-free N2, or under vac., or in a vac. dry box under Ar; addn. of phosphide soln. to GaCl3 soln., -78°C, allowed to warm slowly, stirred, room temp.; evapn. (vac.), extn. (hexane), filtration, concd. (reduced pressure), cooled, collected, dried (vac.);

in tetrahydrofuran; toluene byproducts: HP(C(CH3)3)2, P2(C(CH3)3)4; LiP(C(CH3)3)2 suspended in toluene, cooled to -78 °C, GaBr soln. in 3:1 toluene/THF added dropwise, mixt. stirred, warmed to room temp. over 6 h, soln. heated to 50 °C for 1 h under reduced pressure; soln. filtered, solvent removed (vac.), residue redissolved (toluene), filtered, toluene extract stored at 7 °C for crystallization for several weeks;

in tetrahydrofuran; toluene soln. of GaBr in toluene/THF (3:1) warmed from -78 °C to -35 °C; slight excess of LiP(C(CH3)3)2 suspended in toluene added; react.mixt. warmed to room temp. over 10 h; then held at 60 °C for 2 h; crystd. over several days in drying oven (50 °C);

in 1,4-dioxane T=40°C;

in tetrahydrofuran byproducts: LiCl; to a soln. of LiP(t-Bu)2 in THF equimolar HgCl2 was added slowly; product pptd.;