1: sodium tetrafluoroborate; 3,5-bis(trifluoromethyl)phenyl bromide With magnesium; ethylene dibromide in diethyl ether T=20°C; Heating / reflux; 2: sodium carbonate in diethyl ether; water 0.5 h;

iodine; magnesium in diethyl ether under N2; a soln. of 3,5-(CF3)2C6H3Br in (CH3CH2)2O was added to (CH3CH2)2O containing Mg and I2, the mixt. was refluxed for 1 h, NaBF4 was added, the soln. was stirred for 48 h; Brookhart, M.; Grant, B.; Volpe, A. F., Jr. Organometallics 1992, 11, 3920; Na2CO3 was added, the soln. was stirred (20 min), the ppt. was filtered,the soln. was extd. with (CH3CH2)2O, dried under Na2SO4, treated with d ecolorant C, the solvent was removed, the solid was washed with CH2Cl2, recrystd. (CH2Cl2/C6H14); elem. anal.;

1: With iodine; magnesium in diethyl ether 1 h; Heating; 2: With sodium tetrafluoroborate in diethyl ether 48 h; Further stages.;

in dichloromethane (N2 or Ar); a soln. of Fe complex added to a suspn. of B complex at -78°C, warmed to 20°C over 30 min, stirred for 3 h; filtered, layered with hexanes;

in tetrahydrofuran under N2 or Ar; THF added to solid mixt. of Fe complex and NaB(C6H3(CF3)2)4; THF soln. of In compd. added; volatiles removed; extd. into toluene; soln. filtered; layered with hexane; crystd. for 1 wk; elem. anal.;

in THF-d8 (tetrahydrofuran-d8) byproducts: NaCl; (Ar); addn. of cold THF-d8 soln. of gold compd. and borate deriv. to cold THF-d8 soln. of platinum compd. at -30°C, stirring at -30°C for 15 min and at room temp. for 1 h; filtration, cooling to -30°C, filtration, chromy. (silica gel, CH2Cl2), elem. anal.;

in benzene-d6 byproducts: sodium triflate; (inert atm.); addn. of boron compd. to a soln. of platinum complex in C6D6; filtration, concn., crystn., X-ray diffraction;

in dichloromethane; toluene (N2); imdazole was added to soln. of ReBr(CO)5 in toluene, refluxed for 30 min, evapd. in vac., dissolved in CH2Cl2, AgOTf was added, stirred inthe dark for 1 h, filtered through celite, NaBAr'4 and pyridine were ad ded, stirred for 1 h; filtered, concd., precipitated with hexane, washed with hexane, elem. anal.;

in dichloromethane; toluene (N2); imdazole was added to soln. of ReBr(CO)5 in toluene, refluxed for 30 min, evapd. in vac., dissolved in CH2Cl2, AgOTf was added, stirred inthe dark for 1 h, filtered through celite, NaBAr'4 and pyridine were ad ded, stirred for 1 h; filtered, concd., precipitated with hexane, washed with hexane, elem. anal.;

in dichloromethane; toluene (N2); imdazole was added to soln. of ReBr(CO)5 in toluene, refluxed for 30 min, evapd. in vac., dissolved in CH2Cl2, AgOTf was added, stirred inthe dark for 1 h, filtered through celite, NaBAr'4 and pyridine were ad ded, stirred for 1 h; filtered, concd., precipitated with hexane, washed with hexane, elem. anal.;