Method of removing transition metals.

Abstract

The present invention generally relates to the discovery that the soly. of metal complexes may be readily manipulated by the addn. of one or more soly.-enhancing compds. This manipulation of the solubilities allows for the prepn. of suitable samples for precise quant. anal. and for the facile purifn. of the desired products from the reaction mixt. contg. one or more metal complexes. In one embodiment of the invention, the relative solubilities between two solns. are manipulated so as cause the metal complex found in a first soln. to transfer to a second soln. that is generally immiscible with the first soln. The metal complex is thus sepd. from the reaction mixt. which comprises the first soln. by the removal of the second soln. In another embodiment, the soly.-enhancing compds. of the present invention is used to prep. samples contg. metal complexes for precise quant. anal. such as inductively coupled plasma mass spectroscopy. Thus, Cl2Ru(PPh3)2(:CHPh) mediated ring-closing metathesis of di-Et diallylmalonate in CH2Cl2 gave a soln. of di-Et 3-cyclopentene-1,1-dicarboxylate which was dild. with Et vinyl ether. Typical purifn. procedure involves the addn. of above soln. with a soln. of P(CH2OH)3 in CH2Cl2 contg. Et3N and finally addn. of water. The aq. layer was sepd. and CH2Cl2 layer gave pure di-Et 3-cyclopentene-1,1-dicarboxylate as yellow oil. [on SciFinder(R)]