反应详情

At 0° C. a solution of 14.2 g of diethyl 2-(p-tolyl)-malonate in 50 ml of methanol was slowly added to a solution of 9.4 g of sodium methylate in 300 ml of methanol. Upon completion of the addition the reaction mixture was allowed to warm up and 5.4 g of formamidine hydrochloride was added. The mixture was stirred at room temperature for 16 h. The solvent was removed under reduced pressure and the remaining residue was treated with 150 ml of 2 N hydrochloric acid. The suspension was stirred for 0.5 h. At 0-5° C., the pH was carefully adjusted to 4 using 10 N sodium hydroxide solution. The precipitate was collected, washed with cold water, isopropanol, and diethyl ether and dried under high vacuum at 65° C. to give 11.2 g of 4,6-dihydroxy-5-(p-tolyl)-pyrimidine (or a tautomer) as a white powder.

1. additionUpon completion of the addition the reaction mixture
2. temperatureto warm up
3. customThe solvent was removed under reduced pressure
4. additionthe remaining residue was treated with 150 ml of 2 N hydrochloric acid
5. stirringThe suspension was stirred for 0.5 h
6. customAt 0-5° C.
7. customThe precipitate was collected
8. washwashed with cold water, isopropanol, and diethyl ether
9. customdried under high vacuum at 65° C.