Method of manufacturing a ruthenium complex
A method of making an alkali metal salt of trans-[tetrachlorobis(1H-indazole)ruthenate (III)] is disclosed.
1. A method of making the compound M[tetrachlorobis(1H-indazole)ruthenate (III)], wherein M is an alkali metal cation, comprising the steps of,
reacting, in an aqueous solution or a mixture of an aqueous solution and a first organic solvent which is water soluble, indazolium trans-[tetrachlorobis(1H-indazole)ruthenate (III)] with an inorganic salt of said alkali metal cation M, to form the compound M[tetrachlorobis(1H-indazole)ruthenate (III)] and an inorganic salt of indazole; and
removing said indazole from said M[tetrachlorobis(1H-indazole)ruthenate (III)] by extraction with a second organic solvent which is not substantially water soluble.
2. A method of making the compound M[tetrachlorobis(1H-indazole)ruthenate (III)], wherein M is an alkali metal cation, comprising:
dissolving indazolium trans-[tetrachlorobis(1H-indazole)ruthenate (III)] in an aqueous solution or a mixture of an aqueous solution and a first organic solvent which is water soluble;
reacting said indazolium trans-[tetrachlorobis(1H-indazole)ruthenate (III)] with an inorganic salt of said alkali metal cation M to form the compound M[tetrachlorobis(1H-indazole)ruthenate (III)] and an inorganic salt of indazole; and
extracting said indazole from said M[tetrachlorobis(1H-indazole)ruthenate (III)] with a second organic solvent which is not substantially water soluble.
3. The method of claim 2 , wherein M is sodium, and said inorganic salt of said alkali metal cation M is sodium dihydrogenphosphate.
4. A method of making the compound sodium trans [tetrachlorobis(1H-indazole)ruthenate (III)], comprising the steps of,
reacting, in an aqueous solution optionally in admixture with a first organic solvent which is water soluble, indazolium trans-[tetrachlorobis(1H-indazole)ruthenate (III)] with an inorganic salt of sodium, to form the compound sodium trans [tetrachlorobis(1H-indazole)ruthenate (III)] and an inorganic salt of indazole; and
removing said indazole from said sodium trans [tetrachlorobis(1H-indazole)ruthenate (III)] by extraction with a second organic solvent which is not substantially water soluble.
5. A method of making the compound sodium trans [tetrachlorobis(1H-indazole)ruthenate (III)], comprising the steps of,
(1) reacting, in an aqueous solution optionally in admixture with a first organic solvent chosen from acetone or THF or a mixture thereof, indazolium trans-[tetrachlorobis(1H-indazole)ruthenate (III)] with NaH 2 PO 4 , to form the compound sodium trans [tetrachlorobis(1H-indazole)ruthenate (III)] and a dihydrophosphate salt of indazole;
(2) removing said indazole from said sodium trans [tetrachlorobis(1H-indazole)ruthenate (III)] by extraction with CH 2 Cl 2 ;
(3) extracting the sodium trans [tetrachlorobis(1H-indazole)ruthenate (III)] resulted from step (2) with ethyl acetate under saturation with NaCl; and
(4) precipitating the sodium trans [tetrachlorobis(1H-indazole)ruthenate (III)] from step (3) by addition of diethyl ether.