Sodium acetate (3.3 g) was dissolved in concentrated aqueous ammonia (40 mL of 30%). Na2Fe(CN)5NO.2H2O (10.0 g) was added to produce a red solution. The mixture was stirred vigorously at ice bath temperature for 1.25 hours, during which time a yellow solid formed. The mixture was refrigerated for 5 hours, and was then filtered cold. The yellow product was taken up in about 20 mL of cold water and the mixture was filtered. The yellow-orange filtrate was poured rapidly into an equal volume of absolute ethanol, resulting in the formation of a canary-yellow solid. The mixture was filtered, and the product was washed twice with 10-mL portions of ethanol and suctioned dry. The product was then transferred to a beaker and dried over CaSO4 in a desiccator overnight.
2.0 g of sodium pentacyanoammineferrate(3-) were slurried a cold mixture of 7 mL of water and 7 mL of DMSO, and the mixture was stirred at ice bath temperature for 30 minutes. After all solid had dissolved, 50 mL of ethanol saturated with NaI was added rapidly, and the bottom of the flask was scratched vigorously with a stirring rod. The product was collected by suction filtration, washed with ethanol, and suction dried. The product was purified by dissolving it in a minimum volume of water and reprecipitating it using NaI-saturated ethanol.
1 mmole Na3Fe(CN)5(NH3).2H2O and 1 mmole N-methylpyrazinium iodide (g) were weighed into a 50-mL Erlenmeyer. A minimum volume (5 mL) of water was added to dissolve the reagents, and the solution was allowed to stand for several minutes until the intense blue color had fully developed. Approximately 15-20 mL ethanol was then added to the rapidly stirred solution using a Pasteur pipet. The mixture was then refrigerated for 30 minutes. The blue crystals were isolated by suction filtration, washed with ethanol, and suction dried.