反应详情

To N-[1-(1-Benzyl-4,5-dimethyl-6-oxo-1,6-dihydro-pyrimidin-2-yl)-2-methyl-propyl]-N-[4-(1,3-dioxo-1,3-dihydro-isoindol-2-yl)-2-oxo-butyl]-4-methyl-benzamide (0.884 g, 1.62 mmol) in glacial acetic acid (15 mL) was added ammonium acetate (6.22 g, 80.8 mmol) and the reaction was heated at reflux for 16 h. The reaction was concentrated in vacuo and the residue was basified with saturated NaHCO3, extracted into EtOAc, washed with water and brine, dried (Na2SO4), and evaporated to dryness. The residue was purified by flash chromatography on silica gel (3:1 EtOAc:hexanes) to give the title compound as a pale yellow foam (0.371 g, 38%). MS(ES+) m/c 600 [M+H]+.

1. temperaturethe reaction was heated
2. temperatureat reflux for 16 h
3. concentrationThe reaction was concentrated in vacuo
4. extractionextracted into EtOAc
5. washwashed with water and brine
6. dry with materialdried (Na2SO4)
7. customevaporated to dryness
8. customThe residue was purified by flash chromatography on silica gel (3:1 EtOAc:hexanes)