Toxicity synthesis methods with little

The total time required for the synthesis and isolation of the product is 4-5 hr. It is prepared by a modification of the method of Liu, Liu, and Bailar. A suspension of [Ru(bpy)2Cl2]-2H20 (0.5 g, 0.46 mmol) in 2 M HCl (50 mL) contained in a 250-mL conical flask is warmed to 80° on a steam bath in a well-ventilated fume hood. Chlorine gas is bubbled through the solution via a Pasteur pipette. ( Caution. Chlorine gas is toxic and corrosive. This operation must be performed in a well-ventilated fume hood.) The bubbling is continued until all the solid dissolves leaving a red solution. Concentrated aqueous HCl (36%, 15 mL) is added cautiously, and the solution is allowed to cool for 1 hr. ( Caution. Hydrogen chloride is toxic and corrosive, and therefore the operation is performed in a fume hood.) After further cooling in an ice bath for 2 hr, the crystals are collected on a medium-porosity filter, washed with a little cold HCl (5 M, 5 mL), dried under vacuum, and then washed with diethyl ether (3 x 10 mL). Yield 0.48 g (90%). 

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