反应详情

温度

0 °C

To a suspension of hydroxy-[4-(4-isopropyl-piperazine-1-carbonyl) -phenyl]-methanesulfonic acid sodium salt (49.0 g, 135 mmol) in de-ionized H2O (490 mL) at 0° C. was added 1 N NaOH (100 mL) in 10 mL portions with vigorous stirring. A clear solution resulted (pH 12), which was stirred at 0° C. for 1 h, then at room temperature for 30 min. The aqueous solution was extracted with EtOAc (3×200 mL), followed by CH2Cl2 (3×200 mL). The organic layers were combined, washed with brine (1×300 mL), dried (Na2SO4) and concentrated to yield the title compound as a pale yellow oil.

1. customA clear solution resulted (pH 12), which
2. waitat room temperature for 30 min
3. extractionThe aqueous solution was extracted with EtOAc (3×200 mL)
4. washwashed with brine (1×300 mL)
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated