Sodium Hydroxide → 4,4'-Dichloro-2,2'-bipyridine

Participants

Reaction Conditions

Reaction Steps

2 mL of chloroform, 0.326 mL of phosphorus trichloride and 0.082 g of 4,4′-dichloro-2,2′-bipyridyl-N,N′-dioxide were added to a 100 mL round bottom flask equipped with a condenser, and the mixture was refluxed in a hot water bath for 75 hours. The reaction solution was cooled with ice, poured into crushed ice and neutralized with 25% NaOH to pH 7 or higher. Chloroform was removed from the solution by distilling off under reduced pressure. The precipitated white powder was collected by filtration and washed with water. The powder was dissolved in a small amount of petroleum ether and recrystallized in a refrigerator overnight to give white needle crystal. The crystal was dried by heating to 60° C. under reduced pressure to give 4,4′-dichloro-2,2′-bipyridine.

Provenance & Evidence