反应详情

温度

60 °C

{3-[2-Fluoro-5-(4-oxo-3,4-dihydro-phthalazin-1-ylmethyl)-phenyl]-5-methyl-2,4-dioxo-imidazolidin-1-yl}-acetic acid methyl ester (39)(0.03 g, 0.068 mmol) was dissolved in solution of 7N ammonia in methanol (2 ml, 14 mmol) and placed in a sealed tube. The reaction was then heated to 60° C. for 18 hours. The resultant solution was concentrated in vacuo absorbed onto a 1 ml silica cartridge. The material was eluted with neat ethyl acetate. RF of 0.65 yielding pure amide product. Single peak in LC-MS, (8 mg, 100% purity) and required no further purification; m/z (LC-MS, ESP), RT=2.84 mins (M+H) 424;

1. customplaced in a sealed tube
2. concentrationThe resultant solution was concentrated in vacuo
3. customabsorbed onto a 1 ml silica cartridge
4. washThe material was eluted with neat ethyl acetate
5. customno further purification