反应详情

温度

120 °C

To a solution of 3-(4-bromo-phenyl)-2-cyano-3-(2,4-difluoro-phenyl)-propionic acid ethyl ester (2.4 g) in acetic acid (11 mL) was added water (6 mL) and concentrated H2SO4 (6.83 mL) at 0° C. The reaction mixture was heated to 120° C. overnight, then cooled and poured on ice and extracted with ethyl acetate (3×100 mL). The organic layers were washed with brine, dried over magnesium sulfate, filtered and concentrated in vacuo. The crude reaction product was purified by silica gel chromatography using a MPLC system (CombiFlash Companion, Isco Inc.) eluting with a gradient of n-heptane/ethyl acetate (1:0 to 1:1) to provide the title compound as an off-white solid. MS (ESI−): m/z=339.0 ([M−H]−).

1. temperaturecooled
2. additionpoured on ice
3. extractionextracted with ethyl acetate (3×100 mL)
4. washThe organic layers were washed with brine
5. dry with materialdried over magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customThe crude reaction product
9. customwas purified by silica gel chromatography
10. washeluting with a gradient of n-heptane/ethyl acetate (1:0 to 1:1)