反应详情

温度

120 °C

(S)-1-(4-Chloroquinolin-7-ylmethyl)-4-[3-(5-chlorothiophen-2-yl)-allyl]-3-methylpiperazin-2-one(0.35 g, 0.82 mmol) is treated with phenol (2 g) and ammonium acetate (0.7 g, 9.1 mmol) and heated to 120° C. in a sealed vessel for 1 hour. Upon cooling, the solution is partitioned between 2 N NaOH and ethyl acetate. The organic layer is separated and washed with fresh 2 N NaOH (3×100 mL) and water. The organic layer is concentrated and the residue is purified by reverse phase HPLC to give the title compound as a white solid (0.15 g, 0.35 mmol). MS (ISP) m/z 427, 429, (M+H), Cl pattern.

1. temperatureUpon cooling
2. customthe solution is partitioned between 2 N NaOH and ethyl acetate
3. customThe organic layer is separated
4. washwashed with fresh 2 N NaOH (3×100 mL) and water
5. concentrationThe organic layer is concentrated
6. customthe residue is purified by reverse phase HPLC