Hydrogen Bromide → HCID 70004542, compound

Participants

Reaction Steps

A mixture of intermediate 15 (55 g) and hydrobromic acid (48%) (55 g) in methanol (700 ml) was hydrogenated with palladium on activated carbon (10%) (5 g) as a catalyst. After completion, the precipitate was filtered off and the filtrate evaporated. Ammonium hydroxide was added to the residue which was subsequently extracted with CHCl3. The separated organic layer was dried and evaporated. The residue was purified by column chromatography over silica gel (eluent: CHCl3 /CH3OH 90/10). The pure fractions were collected, the solvent was evaporated and the residue was recrystallized from 4-methyl-2-pentanone, yielding 17 g (44%) of (±)-6,7,8,9-tetrahydro-3-(2-bromoethyl)-9-hydroxy-2-methyl-4H-pyrido[1,2-a]pyrimidin-4-one (intermediate 16).

Provenance & Evidence