反应详情

温度

90 °C

Anhydrous hydrazine (0.30 mL, 9.6 mmol) was added via syringe to a solution of the intermediate of Step B (4.8 mmol) in glacial acetic acid (6 mL) under a nitrogen atmosphere. The reaction was heated at 90° C. for 30 minutes, then cooled and concentrated in vacuo to a light brown solid. The solid was redissolved in aqueous methanol and the solution neutralized with saturated aqueous sodium bicarbonate. The mixture was extracted with dichloromethane and ethyl actate, the extracts were combined and dried over sodium sulfate. Evaporation of the solvents yielded a solid which was triturated with ether to provide the title product (0.81 g) as an off-white solid, m.p. 196-198° C.

1. temperaturecooled
2. concentrationconcentrated in vacuo to a light brown solid
3. dissolutionThe solid was redissolved in aqueous methanol
4. extractionThe mixture was extracted with dichloromethane and ethyl actate
5. dry with materialdried over sodium sulfate
6. customEvaporation of the solvents
7. customyielded a solid which
8. customwas triturated with ether