Sulfuric Acid → HCID 135730618, compound

Participants

Reaction Steps

A mixture of 3-bromo-5-(2-ethoxy-5-ethynyl-3-pyridinyl)-2-methyl-2,6-dihydro-7H-pyrazolo[4,3-d]pyrimidin-7-one (Example 57) (750 mg, 2 mmol), 1N H2SO4 (2 mL) and HgSO4 (50 mg, 0.17 mmol) in acetone (25 mL) was stirred at reflux for 10 h then at room temperature for 14 h. Further H2SO4 (5 mL of 1 N) was added and refluxing was continued for a further 4 h. The mixture was cooled and the solvent evaporated and the residue partitioned between dichloromethane and water. After basifying with solid sodium bicarbonate a white precipitate formed which was filtered off before separating the phases. The organic layer was dried (MgSO4), concentrated and combined with the solid previously filtered to give the title compound as a poorly soluble solid.

Provenance & Evidence