Hydrochloric Acid → Benzenediazonium, 4-methoxy-, hexafluorophosphate(1-)

Participants

Reaction Conditions

Reaction Steps

1440 cc. of 5N aqueous hydrochloric acid was charged into a 3000 cc. capacity vessel equipped with a stirrer, thermometer, condenser and addition funnel. 184.5 g. (1.5M) of p-anisidine was added and the mixture stirred at room temperature until complete conversion to the ammonium salt was achieved. The solution was cooled in an ice-methanol bath to -5° C. Diazotization was achieved by adding 184.5 g. (1.52M) of sodium nitrite in 300 ml of water dropwise over a 30-minute period while maintaining the temperature between 0°-5° C. A solution of 244.5 g. (1.5M) of ammonium hexafluorophosphate in 300 ml of water was added to precipitate the hexafluorophosphate salt. The salt was filtered, washed chloride-free and vacuum-dried at 25° C.

Provenance & Evidence