反应详情

The above-prepared dioxoimidazolidine-1-acetate product of paragraph (2) (15 g) was suspended in a mixed solvent of acetic acid and hydrochloric acid and the mixture was heated to reflux with stirring for two hours. Then the mixture was concentrated in vacuo, ether-chloroform was added thereto. The crystals were dislodged from the wall of the reaction flask with a spatula. The solid was washed with ether and recrystallized from a mixed solvent of ethanol and water to give 8.1 g of 5-hydroxy-3-(3-nitrobenzyl)-2,4-dioxoimidazolidine-1-acetic acid [Compound 15]. The melting point, MS, IR, NMR, and elementary analysis for the compound were:

1. temperaturethe mixture was heated
2. temperatureto reflux
3. concentrationThen the mixture was concentrated in vacuo, ether-chloroform
4. additionwas added
5. washThe solid was washed with ether
6. customrecrystallized from a mixed solvent of ethanol and water