1: chlorodi-tert-butylphosphine With lithium aluminium tetrahydride in diethyl ether T=20°C; CoolingInert atmosphere; 2: borane in tetrahydrofuran T=0 - 20°C;

1: With lithium aluminium tetrahydride in diethyl ether T=20°C; Inert atmosphereCooling; 2: With borane in tetrahydrofuran T=0 - 20°C; Inert atmosphere;

dimethylsulfide borane complex in toluene T=23°C; Inert atmosphere;

in tetrahydrofuran (N2); BH3*THF in THF added slowly at room temp. to tBu2PH in THF, stirred for 1 h; evapd. (vac.), dissolved in n-pentane, crystd. at 0°C for 7 d;

in N,N-dimethyl-formamide P compd. added dropwise to a soln. of NaBH4 at 0°C, allowed to warm to room temp. and stirred for 16 h; H2O and Et2O added, the aq. layer extd. (Et2O), the combined org. phase washed (H2O, brine), dried (MgSO4), evapd., recrystd. (hexane); elem. anal.;

in tetrahydrofuran 60 h; Cooling with iceSchlenk technique;

1: rhodium(III) chloride (hydrated) / neat (no solvent) 2: neat (no solvent) View Scheme

1: rhodium(III) chloride (hydrated) / neat (no solvent) 2: neat (no solvent) View Scheme