in benzene chromatography (Al2O3, CHCl3/CH3OH), dissolving in toluene and pptn.;;

1: diethyl ether 2: (dehydration) 3: (bromination) 4: benzene View Scheme

1: (dehydration) 2: (bromination) 3: benzene View Scheme

1: (bromination) 2: benzene View Scheme

n-butyllithium; N,N,N',N,-tetramethylethylenediamine in diethyl ether; hexane addn. of 1 equiv. BuLi (in hexane) to amine and TMEDA (1 equiv.) in Et2O, stirring (8 h, room temp.), slow mixing with B(OMe)3 in Et2O (<-60°C, <1 h), slow warming to room temp. (during 24 h); evapn., CH2Cl2 addn., filtration, H2O addn. to filtrate, evapn., distn.off of water with toluene, recrystn. (toluene);

in not given according to: H. R. Snyder, M. S. Konecky, and W. J. Lennars, J. Am. Chem. Soc., 80, 3611(1958), and R. T. Haekins and H. R. Snyder, J. Am. Chem. Soc., 82, 3863(1960);