Student Synthesis of Tris(ethylenediamine)cobalt(lll) chloride

In spite of the importance of coordination compounds in modern inorganic chemistry few experiments suitable for a 3-hr
laboratory period are available in this area. Cobalt(III) complexes, so important to the development of coordination theory,
generally require a time-consuming air oxidation step in their synthesis and consequently are rarely encountered in the
undergraduate laboratory. We have developed a much more rapid synthesis of tris(ethylenediamine)cobalt(III) chloride
than the customary approach;1 this experiment is quite suitable for inclusion in an undergraduate laboratory.
Procedure. Dissolve 12.0 g CoCl2*6 H2O in 35 ml water; while this is dissolving add 9.0 ml of anhydrous ethylenediamine
to 25 ml water, cool in ice and add 8.5 ml 6 N HC1. Add the C0CI2 solution to the partially neutralized ethylenediamine and
then add 10 ml of 30% H2O2 with stirring. Stir for a few minutes until effervescence ceases, place the mixture on a hot plate
and boil gently.
When the solution has evaporated to a volume of 60 ml, an equal volume of cone, hydrochloric acid is added followed
by 120 ml ethanol. Cool in ice and filter, washing with two portions of ethanol and two portions of ether. Air dry.
Results. Following this procedure students obtain approximately 10 g of the complex; evaporation to lower volumes
does not afford significant improvement while evaporation to very low volume (20-30 ml) gives a large amount of a green
impurity. During the evaporation we have students synthesize tris(ethylenediamine)nickel(II) chloride. They can then
compare the two (e.g., lability in acid).

Broomhead, J. A., Dwyer, F. P., and Hogarth, J. W., Inorg. Syn., 6,183 (1960).
1

University of Connecticut Ronald A. Krause

Storrs, 06268 Elizabeth A. Megargle
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Volume 53, Number 10, October 1976 / 667