反应详情

19-2 (1.59 g, 4.89 mmol) was suspended in 25 mL MeOH. Upon addition of hydrazine (2.0 mL, 64 mmol) the reaction became homogeneous. After 20 h a heavy precipitate had formed. The pH was adjusted to 1 by addition of 6N HCl, MeOH evaporated, and the solid suspended in 1N HCl. After filtering through Celite, the filtrate was washed with CH2Cl2, the pH was adjusted to 12 with 6N NaOH. The aqueous layer was extracted with fresh CH2Cl2. This organic phase was dried (Na2SO4) and concentrated providing 19-3 as a white solid.

1. customAfter 20 h a heavy precipitate had formed
2. customevaporated
3. filtrationAfter filtering through Celite
4. washthe filtrate was washed with CH2Cl2
5. extractionThe aqueous layer was extracted with fresh CH2Cl2
6. dry with materialThis organic phase was dried (Na2SO4)
7. concentrationconcentrated