反应详情

The above-prepared dioxoimidazolidine-1-acetate product of paragraph (2) from several production runs (1.7 g) was heated to reflux in a mixed solvent of 12 mL of acetic acid and 4 mL of concentrated hydrochloric acid for one hour. After evaporating the solvent therefrom, 12 mL of acetic acid and 4 mL of concentrated hydrochloric acid were added to the residue and the mixture was heated to reflux for one hour more. The refluxed mixture was poured over a mixed solution of ethyl acetate and 10% sodium hydroxide, the mixture was extracted with 10% sodium hydroxide several times and the resulting aqueous extract was subjected to a reverse extraction several times. The extracts were combined, dried over sodium sulfate, concentrated and recrystallized from ethanol to give 350 mg of 3-(3-nitrobenzyl)-2,4-dioxoimidazolidine-1-acetic acid [Compound 6]. The melting point, MS, IR, NMR, and elementary analysis for the compound were:

1. customAfter evaporating the solvent
2. addition12 mL of acetic acid and 4 mL of concentrated hydrochloric acid were added to the residue
3. temperaturethe mixture was heated
4. temperatureto reflux for one hour more
5. additionThe refluxed mixture was poured over a mixed solution of ethyl acetate and 10% sodium hydroxide
6. extractionthe mixture was extracted with 10% sodium hydroxide several times
7. extractionthe resulting aqueous extract
8. extractionwas subjected to a reverse extraction several times
9. dry with materialdried over sodium sulfate
10. concentrationconcentrated
11. customrecrystallized from ethanol