n-butyllithium; N,N,N',N,-tetramethylethylenediamine in hexane under N2; TMEDA is added to ferrocene in hexane, n-BuLi is added dropwise with stirring, stirred at room temperature overnight; the solid is dissolved in hexane, HCl is added, the solid is filtd., washed (hexane);

tert.-butyl lithium in tetrahydrofuran; n-heptane under N2; tBuLi in hexane is added to ferrocene in THF at -20°C, stirred for 30 min, DMF is added at -10°C, HCl is added; extd. with CH2Cl2, chromd. (SiO2, CH2Cl2);

n-butyllithium; N,N,N',N,-tetramethylethylenediamine in diethyl ether; hexane Ar; ferrocene (53.8 mmol) suspnd. in hexane, hexane soln. of BuLi (107.5mmol) added, TMEDA (55.7 mmol) added dropwise, stirred at room temp. fo r 14 h, Et2O soln. of ligand (104.1 mmol) added dropwise, stirred for 30min; extd. (H2O), reextd. (CH2Cl2), org. layer washed (aq. HCl), dried (MgSO4), filtered, concd., chromd. (SiO2, CH2Cl2/hexane=1/1), dried;

1-methyl-piperazine; tert.-butyl lithium in tetrahydrofuran; pentane (argon); addn. of t-BuLi/pentane to N-methylpiperazine/THF/r.t., stirring (15 min), addn. of Fe(C5H5)(C5H4CHO)/THF, stirring (r.t., 2 h), -> 0°C, addn. of t-BuLi/pentane (1 h), -> -78°C, addn. of DMF (-78°C to r.t.), hydrolysis; extn. (CH2Cl2), flash chromy. (SiO2; pentane/Et2O); 17 percent combined yield (6i:7i = 90:10);

in not given according to J. Organomet. Chem., 1991, 412, 381; org. phase dried over MgSO4, chromy. (silica gel, hexane, then hexane/CH2Cl2 (1/1), and finally CH2Cl2); collection of red band; removal of solvent under reduced pressure, dried under vac.;

t-BuLi or MeLi in diethyl ether; pentane absence of air: addn. of t-BuLi or MeLi (in pentane) to Fe-complex soln.(in ether) at -78°C, stirring for 15 min, then at room temp. for 2 h, cooling to -78°C, addn. of Sn-compd., stirring (-78° C, 15 min, room temp., 1 h); addn. of isopropylamine, H2O, extn. into ether, washing (H2O), drying (MgSO4), evapn., chromy. (SiO2, cyclohexane/ether); diastereomer mixt. notsepd., detd. by (1)H-NMR spectroscopy; yield depending on amt. of MeLi; elem. anal.;

in not given one-pot react. of dilithioferrocene-tmeda complex with DMF; flash chromy. on silica gel;

trichlorophosphate in not given Vilsmeyer formylation;;

tert.-butyl lithium in tetrahydrofuran N2-atmosphere; dropwise addn. of t-BuLi to mixt. of metallocenes at -74 to -70°C, stirring at -30°C for 3 h, addn. of excess DMF, warming to -10°C; water addn., solvent removal (reduced pressure), extn. into CH2Cl2, drying (MgSO4), chromy. (SiO2, hexane, then CH2Cl2, then CH2Cl2/Et2O=1:1);

ammonia; zinc(II) chloride in tetrahydrofuran; diethyl ether; water stirring (room temp., 10 h), Et2O and NH3(aq) addn.; extg. (Et2O), drying (Na2SO4), evapn., chromy. (SiO2, hexanes / Et2O = 9: 1);