Hydrogen Bromide → HCID 178515897, compound

Participants

Reaction Steps

A mixture of 56 (7.4 g, 0.021 mol) and 10% NaOH (200 ml) was heated at reflux with stirring. After 4 hours, the solution was cooled, extracted with CH2Cl2 (2 X), acidified with concentrated HC1, cooled and filtered to yield 100% of crude acid. The crude acid (6.9 g, 0.021 mol), AcOH (40 ml) and 48% HBr (160 ml) were heated at reflux with stirring. After 15 hours, the solution was concentrated to dryness and the residue treated with NaHCO3. The mixture was concentrated to dryness and the residue combined with silica gel and chromatographed on silica gel and the product eluted with 5% CH3OH-CHCl3 to yield 3.0 g (53%) of 57, m.p. 225°-27° C. (CH3CN). Analysis calculated for C9H6N2BrC10.

Provenance & Evidence