Sulfuric Acid → HCID 86631108, compound

Participants

Reaction Conditions

Reaction Steps

6-Amino-1-(pyridin-2-ylmethyl)-2-thioxo-2,3-dihydro-1H-pyrimidin-4-one (0.60 g, 2.56 mmol, obtained from Example 1(b)) was dissolved in acetic acid (90% aq., 10 mL) and was heated at 75° C. for 5 minutes. Sodium nitrite (0.20 g, 2.95 mmol) was added and heating was continued for another 30 minutes. The solvent was removed in vacuo and the residue was suspended in water (6 mL), and ammonia (32% aq., 6 mL) was added. The reaction mixture was heated at 75° C. and sodium dithionite (1.1 g, 6.4 mmol) was added and the resulting mixture was continued stirring at 75° C. for 5 minutes, and then stirred at r.t. for 30 minutes. After adjusting the solution to neutral pH with 2M sulfuric acid the precipitated solid was collected by filtration, washed with a small amount of water and dried, giving the title compound (0.331 g, 52%) as a solid. The crude product was used in the next step without further purification.

Provenance & Evidence