反应详情

To a refluxing mixture of cyclopropane-1,1-dicarboxylic acid (4-benzyloxy-phenyl)-amide (4-fluoro-phenyl)-amide (46 g, 113 mmol), 10% Pd/C (2 g) in EtOH (400 mL) was added dropwise 1,4-cyclohexadiene (62.7 mL, 678 mmol). Stirring was continued for 2-5 h until the reaction was complete. The mixture was cooled to rt, filtered through celite, and washed with EtOH . . . . The solution was then concentrated under reduced pressure. To the flask containing the crude product was added CHCl3 (200 mL). The resulting suspension was stirred for 15 min at rt. The solid was filtered, and dried in the air to give cyclopropane-1,1-dicarboxylic acid (4-fluoro-phenyl)-amide(4-hydroxy-phenyl)-amide (34.4 g, 95%, yield).

1. filtrationfiltered through celite
2. washwashed with EtOH
3. concentrationThe solution was then concentrated under reduced pressure
4. additionTo the flask containing the crude product
5. additionwas added CHCl3 (200 mL)
6. stirringThe resulting suspension was stirred for 15 min at rt
7. filtrationThe solid was filtered
8. customdried in the air