反应详情

Acetic anhydride (11.2 mL, 118.61 mmol) was added to N-hydroxy-2-(1-pyrrolo[2,3-b]pyridin-1-yl-cyclopentyl)-acetamidine (400) (1.8 g, 6.98 mmol) and stirring was continued for 3 h at room temperature (TLC, ethyl acetate, Rf=0.5). Water (50 mL) was added, and the mixture was basified to pH 8 by solid NaHCO3 and extracted with ethyl acetate (3×50 mL). The organic phase was thereafter dried and concentrated. The crude product was purified by Combi-Flash column (eluted at 20-30% ethyl acetate in hexane) to get 2-(1-{1H-pyrrolo[2,3-b]pyridin-1-yl}cyclopentyl)ethanimidamido acetate (401) (1.7 g, 81%) as an off-white solid.

1. extractionextracted with ethyl acetate (3×50 mL)
2. customThe organic phase was thereafter dried
3. concentrationconcentrated
4. customThe crude product was purified by Combi-Flash column (eluted at 20-30% ethyl acetate in hexane)