反应详情

温度

100 °C

Under an atmosphere of nitrogen, sodium metal (1.15 g, 0.05 moles) was added portionwise to ethanol (dried over 4 Å molecular sieves, 50 mL) at 40° C. and the mixture stirred until a solution was formed. Urea (3.0 g, 0.05 moles) was added and the mixture heated at 100° C. for 15 minutes until complete dissolution was achieved. The reaction mixture was allowed to cool slightly and methoxymethyl malonate (8.1 g, 0.05 moles) added, a pink/white precipitate forming almost immediately. Further dry ethanol (10 mL) was added to maintain a stirrable mixture. The resultant suspension was heated at 100° C. (reflux) for 4 hours. The reaction mixture was concentrated in vacuo and the residue dried under high vacuum to give 6-Hydroxy-5-methoxy-1H-pyrimidine-2,4-dione, sodium salt as a pink/white solid, used in the subsequent step without analysis or purification.

1. customwas formed
2. temperatureto cool slightly
3. customa pink/white precipitate forming almost immediately
4. temperatureto maintain a stirrable mixture
5. temperature(reflux) for 4 hours
6. concentrationThe reaction mixture was concentrated in vacuo
7. customthe residue dried under high vacuum