Malonic Acid → 1-Benzyl-3-phenylbarbituric acid

In a 300-ml glass flask equipped with a thermometer, a reflux condenser and a stirrer, 5.0 g of N-benzyl-N′-phenylurea synthesized in Exemplary Synthesis 1, 2.5 g of malonic acid, 20 ml of toluene, and 5.6 g of acetic anhydride were put, the content was heated under stirring so as to adjust the inner temperature to 80° C., and kept under stirring at 80° C. for 3 hours. The content was then cooled to 50° C., washed with 15 ml of water, and the aqueous phase was discarded. The organic layer was kept under stirring at room temperature, and 5 ml of isopropanol was dropped therein. The content was further stirred at 10° C. or below for 0.5 hours, filtered under suction to collect a deposited crystal, the crystal was washed with cold isopropanol, and dried, to thereby obtain 4.6 g of 1-benzyl-3-phenylbarbituric acid as an intermediate.

1. temperaturethe content was heated
2. customto 80° C.
3. stirringunder stirring at 80° C. for 3 hours
4. washwashed with 15 ml of water
5. stirringunder stirring at room temperature
6. addition5 ml of isopropanol was dropped
7. stirringThe content was further stirred at 10° C. or below for 0.5 hours
8. filtrationfiltered under suction
9. customto collect a deposited crystal
10. washthe crystal was washed with cold isopropanol
11. customdried

ORD-Eintrag

ord-b8a0fa979ae9477e9cd451768f598491

Quelldatensatz

uspto-grants-2016_02

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09256099B2