反应详情

A solution of (2-{(chloroacetyl) [2-(3-cyano-4-fluorophenyl)ethyl]amino}ethyl)carbamate (0.12 g, 0.31 mmol) and TFA in 5 mL of DCM was stirred at room temperature for 1 h. The solvent was evaporated. The residue was dissolved in 40 mL of ethanol and K2CO3 (0.13 g, 0.93 mmol) was added. The resulting mixture was refluxed under N2 overnight, cooled to room temperature, and filtered. The filtrate was evaporated and the residue was purified with preprep-HPLC to give 2-Fluoro-5-[2-(2-oxopiperazin-1-yl)ethyl]benzonitrile. 1H-NMR (400 MHz, CDCl3) δ: 7.41˜7.44 (m, 2H), 7.07˜7.12 (m, 1H), 3.51˜3.53 (m, 4H), 3.18˜3.22 (m, 2H), 2.99˜3.04 (m, 2H), 2.75˜2.86 (m, 2H).

1. customThe solvent was evaporated
2. dissolutionThe residue was dissolved in 40 mL of ethanol
3. temperatureThe resulting mixture was refluxed under N2 overnight
4. filtrationfiltered
5. customThe filtrate was evaporated
6. customthe residue was purified with preprep-HPLC