sodium hydroxide in chloroform T=0°C; 1 h;

sodium hydroxide in chloroform; water T=0 - 10°C; 1 h;

in diethyl ether all manipulations under N2 atm.; org. compd. added to soln. of Fe compd., stirred overnight at room temp.; volatiles removed in vac., solid redissolved in min. amt. of CH2Cl2, chromy. (silica gel, hexane, hexane/CH2Cl2 (1:1)), first band (red-orange) recrystd. from CH2Cl2/hexane; elem. anal.;

in diethyl ether overnight stirring, (N2); vec. evapn., redissolving in min. amount of CH2Cl2, column chromy. (silicagel, hexane, and hexane/CH2Cl2 in 1:1 v:v ratio), recrystn. (CH2Cl2/hexane), elem. anal.;