Synthesis of Tris(2,2'-bipyridine)ruthenium(II) Tetrafluoroborate
Procedure modified by Jonathan Breitzer and George Lisensky
from John A. Broomhead and Charles G. Young, Inorg. Syn. 28, 338-340
(1990).
Procedure
Wear eye protection
Drying RuCl3 (enough for 35 preparations)
Grind about 3 grams of commercial RuCl3·3H2O
in a mortar and pestle and dry in a 100°C oven for a few hours. The
color will change from dark black to a dark brown.
Preparation of NaH2PO2 from H3PO2 (enough for 35 preparations)
Hypophosphorous acid is monoprotic (two of the hydrogens are attached
directly to phosphorus) with a pKa of 1.1. Use caution when handling.
Add 10 mL of 50 % H3PO2 into a beaker containing
6 mL of water and a stirbar.
Slowly add pellets of NaOH until the pH is
about 6-8. This will require about 3.9 g of NaOH. The final solution is
about 6 M in NaH2PO2.
Preparation of the Ru(II) complex
Dissolve 0.083 g (0.40 mmol) RuCl3·3H2O in 8 mL of water
in a 30-mL beaker equipped with a stirbar. Add 0.188 g (1.204 mmol) 2,2’-dipyridyl
and 0.44 mL of NaH2PO2. Cover the beaker with a watch glass and reflux
for 30 minutes. Add water if necessary to maintain the volume.
Add 0.333 g of NaBF4 dissolved in 1.5 mL of water. Let
the solution cool to about room temperature and then cool in ice; crystals
should form.
