反应详情

At 5° C. 12.7 g of sodium methylate was added portionwise to a solution of 18.9 g of dimethyl-(o-methoxyphenoxy)malonate (Example 1b) in 450 ml of methanol. Upon completion of the addition stirring was continued at room temperature for 30 min followed by the addition of 6 g of formamidine hydrochloride. The mixture was stirred at room temperature for 72 h. Eventually, the solvent was removed under reduced pressure and the remaining residue was suspended in diethyl ether. The solid material was filtered off and dissolved in 100 ml of water. The solution was acidified with conc. hydrochloric acid. A white precipitate formed. The precipitate was collected, washed with water and dried to give 15.1 g of 5-(o-methoxyphenoxy)-4,6-dihydroxy-pyrimidine (or a tautomer) as a white powder.

1. customAt 5° C
2. additionUpon completion of the addition
3. stirringThe mixture was stirred at room temperature for 72 h
4. customEventually, the solvent was removed under reduced pressure
5. filtrationThe solid material was filtered off
6. dissolutiondissolved in 100 ml of water
7. customA white precipitate formed
8. customThe precipitate was collected
9. washwashed with water
10. customdried