反应详情

10 g of diethyl 2-(4,6-dimethoxypyrimidin-2-yl)- 2-isopropylmalonate, 5,0 g of sodium hydroxide, 20 ml of water and 50 ml of methanol were placed in a round bottomed flask, and were stirred under heat-refluxing for 6 hours. The reaction liquor was concentrated, and 100 ml of water was added thereto. The reaction liquor was adjusted to a pH of from 3 to 4 with a dilute hydrochloric acid under cooling with ice, and was extracted twice with 100 ml of diethyl ether. The extracted liquor was washed with water, and was dried with anhydrous sodium sulfate for one night. After filtrating the inorganic salt, the solvent was distilled off under reduced pressure to obtain 5.8 g of a crude crystal. The crude crystal thus obtained was recrystallized from ether-hexane to obtain 5.3 g of the aimed product of white powder (yield=75.1%) having a melting point of 99°-101° C.

1. temperatureunder heat-refluxing for 6 hours
2. concentrationThe reaction liquor was concentrated
3. addition100 ml of water was added
4. temperatureunder cooling with ice
5. extractionwas extracted twice with 100 ml of diethyl ether
6. washThe extracted liquor was washed with water
7. dry with materialwas dried with anhydrous sodium sulfate for one night
8. filtrationAfter filtrating the inorganic salt
9. distillationthe solvent was distilled off under reduced pressure
10. customto obtain 5.8 g of a crude crystal
11. customThe crude crystal thus obtained
12. customwas recrystallized from ether-hexane