反应详情

温度

70 °C

To a solution of {3-[2-fluoro-5-(4-oxo-3,4-dihydro-phthalazin-1-ylmethyl)-phenyl]-5-methyl-2,4-dioxo-imidazolidin-1-yl}-acetic acid (36A)(0.04 g, 0.094 mmol) in methanol (4 ml) was added concentrated sulfuric acid (1 ml) and stirred at 70° C. for 90 minutes before being cooled to room temperature. The reaction mixture was then concentrated in vacuo, diluted with water (10 ml) an extracted with ethyl acetate (2×10 ml). The organic layer was then dried over sodium sulfate and concentrated in vacuo to afford a colourless oil. Single peak in LC-MS, (52 mg, 95% purity) and required no further purification; m/z (LC-MS, ESP), RT=3.24 mins (M+H) 439;

1. temperaturebefore being cooled to room temperature
2. concentrationThe reaction mixture was then concentrated in vacuo
3. additiondiluted with water (10 ml)
4. extractionan extracted with ethyl acetate (2×10 ml)
5. dry with materialThe organic layer was then dried over sodium sulfate
6. concentrationconcentrated in vacuo
7. customto afford a colourless oil
8. customno further purification