Acetic Acid → HCID 131710702, compound

Participants

Reaction Steps

A solution of IV hydrobromide (0.13 m.) in 350 ml. acetic acid was treated dropwise with a solution of bromine (0.13 m) in 50 ml. acetic acid. After stirring for 1/2 hour, the reaction was diluted with 1.5 1. "Skellysolve B" (essentially n-hexane) and cooled. The precipitated residue was separated by decantation and washed with cold "Skellysolve B". The residue was taken up in methylene chloride and treated with dilute ammonium hydroxide until basic. The layers were separated and the aqueous layer extracted two times more with methylene chloride. The combined extracts were dried (MgSO4) and concentrated. The residue was taken up in acetone and allowed to crystallize with stirring. The crystals were collected to give V (69%). The analytical sample was recrystallized from methanol; mp 158°-160° C.

Provenance & Evidence