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

In spite of the importance of cwrdination compounds in modern inorganic chemistry few experiments suitable for a 3-hr
laboratory period are available in this area. Cohalt(II1) 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
. .
undereraduate laboratorv. We have develooed a much more raoid svnthesis of tris(ethvlenediamine~eobalt(II1I
. , .~chloride
~ ~

rhan rhr rusromary approach;' this experiment is quite ~urrahlefor mclusion in an undrrgraduare laboratory
P ~ o c e d ~ r eIYisd\.e 12.0 g C U C ~H20
~ . in
~ 35 ml water; while this is dissolving add D O rnl of onhydrow rthylanediaminc
to25 ml wafw,coul in iccand add 8.5 rnl6.Y HCI.Add theCoClr solutrm rorhe partially nr~traliaederhylenediamine and
then add 10 mlof 3O%H202 withstirring. Stir for a few minutes until effervescence ceases, place themixture o n a hot plate
and bail gently.
When the solution has evaporated to a volume of 60 ml, an equal volume of conc. 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).
University of Connecticut Ronald A. Krause
Storrs, 06268 Elizabeth A. Megargle

Volume 53, Number 10, October 1976 / 687