反应详情

The hydrazino pyrazine (20.20 g, 183 mmol, prepared as in J. Orq. Chem., 27, 3243 (1962)) was added in portions to the 1,3-diketone (34.7 g, 167 mmol, prepared in Example 1, Step A) in glacial acetic acid (400 mL). The reaction was refluxed for 2 hours, concentrated, and partitioned between EtOAc and K2CO3 (aq). The organics were dried (MgSO4) and evaporated to give a brown solid. Recrystallization from hexanes afforded 29.27 g (62%) of a cream colored solid.

1. temperatureThe reaction was refluxed for 2 hours
2. concentrationconcentrated
3. custompartitioned between EtOAc and K2CO3 (aq)
4. dry with materialThe organics were dried (MgSO4)
5. customevaporated
6. customto give a brown solid
7. customRecrystallization from hexanes