反应详情

4-Butyloxybenzamidine hydrochloride (II) (22.9 g, 0.1 mol) and diethyl ethoxymethylenemalonate (III) (23.8 g, 0.1 mol) were suspended in methanol (100 ml), followed by agitating the suspension while keeping it at 10° C., dropwise adding a sodium methoxide-methanol solution, separately prepared by reacting sodium (2.5 g, 0.11 mol) with methanol (200 ml), then agitating the mixture for 2.5 hours, distilling off methanol under reduced pressure, gradually adding 6N-hydrochloric acid till the solution reached a pH of 4, filtering the resulting white precipitate, washing the precipitate with a small quantity of methanol and drying the precipitate to obtain ethyl-2-(4-butyloxyphenyl)-4-hydroxy-5-pyrimidinecarboxylate (IV) 21.9 g) (yield: 69% based on compound (II)).

1. customat 10° C.
2. customseparately prepared
3. stirringagitating the mixture for 2.5 hours
4. distillationdistilling off methanol under reduced pressure
5. additiongradually adding 6N-hydrochloric acid till the solution
6. filtrationfiltering the resulting white precipitate
7. washwashing the precipitate with a small quantity of methanol
8. customdrying the precipitate