反应详情

Ac2O (30 mL) was added to N-hydroxy-2-(3-phenyl-pyridin-2-yl)-acetamidine (160) (5.3 g, 23.35 mmol) at room temperature. A purple colored solution was formed, after a few hours a dark brown solution was formed which was stirred for 6 h at room temperature. Silica thin layer chromatography was performed (100% ethyl acetate, Rf=0.6). Cold water was added, the mixture was extracted with ethyl acetate (3×50 mL), the organic part was dried and concentrated, the crude product was purified by a CombiFlash column (eluted at 50% ethyl acetate in hexane) to get 2-(3-phenylpyridin-2-yl)ethanimidamido acetate (161) (2.7 g, 42.94% pure and 2 g mixture) as a yellow solid.

1. customA purple colored solution was formed, after a few hours a dark brown solution
2. customwas formed which
3. extractionthe mixture was extracted with ethyl acetate (3×50 mL)
4. customthe organic part was dried
5. concentrationconcentrated
6. customthe crude product was purified by a CombiFlash column (eluted at 50% ethyl acetate in hexane)