Potassium Carbonate → HCID 178433707, compound

Participants

Reaction Conditions

Reaction Steps

To a solution of 1-(3-tetrahydrofuranyl)-3-methyl-6-(4-pyridyl)-pyrazolo[3,4-d]pyrimidin-4-amine (1.08 g, 3.6 mmol) in 60% sulfuric acid (30 ml) at -10° C. was added sodium nitrite (5.6 g, 81.2 mmol) in water (8 ml). The reaction mixture was stirred at -5° C. for 2 hours, then at room temperature for 24 hours. The mixture was poured onto ice-water, neutralized with K2CO3 and the salts were collected by filtration. The aqueous filtrate was extracted with chloroform (6×100 ml) and the combined organic layers were concentrated in vacuo. The residue was dissolved in isopropanol, treated with Darco and concentrated in vacuo to afford 0.5 g (46%) of 1-(3-tetrahydrofuranyl)-3-methyl-6-(4-pyridyl)pyrazolo[3,4-d]pyrimidin-4-one.1/4 hydrate as an off-white fluffy powder, m.p. 251° C. when dried at 90° C. for 24 hours in high vacuum.

Provenance & Evidence