反应详情

N-chloro-succinimide (NCS, 79.45 g, 0.6 mol) was added to a solution of compound 7 (25.8 g, 0.12 mol) in dry CH3CN (300 mL). The resulting suspension was heated at reflux for 2 hours and then cooled to room temperature. After washing with 10% aqueous NaOH (2×150 mL), then water (2×200 mL), the organic phase was dried over magnesium sulfate, filtered, and concentrated under reduced pressure to give a solid. This solid was recrystallized from EtOH to give 28.7 g (95%) of compound 8 as a white solid.

1. temperatureThe resulting suspension was heated
2. temperatureat reflux for 2 hours
3. washAfter washing with 10% aqueous NaOH (2×150 mL)
4. dry with materialwater (2×200 mL), the organic phase was dried over magnesium sulfate
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customto give a solid
8. customThis solid was recrystallized from EtOH