反应详情

Scheme IB, step C: A 1000 mL three necked flask equipped with a mechanical stirrer, thermometer, addition funnel and a reflux condenser is charged with (+,−) cis-2-(2-phenyl-cyclopentyl)-isoindole-1,3-dione (27.34 g, 93.91 mmol) and toluene (400.0 mL). To this solution was added anhydrous hydrazine (29.48 mL, 939.09 mmol) dropwise over a period of 15 minutes. Stirred reaction at room temperature for 60 minutes then heated it at 90° C.-95° C. for 6.0 hours. Cooled reaction to room temperature, filtered precipitates, washed cake with toluene (50.0 mL) and concentrated filtrate to provide the title compound as an oil (mass=15.13 g);

1. additionthermometer, addition funnel and a reflux condenser
2. customreaction at room temperature for 60 minutes
3. temperaturethen heated it at 90° C.-95° C. for 6.0 hours
4. temperatureCooled
5. customreaction to room temperature
6. filtrationfiltered
7. customprecipitates
8. washwashed cake with toluene (50.0 mL) and concentrated filtrate