反应详情

To a stirred degassed solution of (161) (2.7 g, 10.04 mmol) in ethanol (135 mL) was added 10% Pd—C (270 mg), the mixture was stirred 16 h under H2 (hydrogen bubbler) at room temperature. Silica thin layer chromatography was performed (ethyl acetate, Rf=0.1). The reaction mixture was filtered through celite, washed with 10% methanol in dichloromethane (5×100 mL), dried and concentrated. The yellow solid was washed with 10% ethyl acetate in hexane (3×30 mL) to get pure 2-(3-phenyl-pyridin-2-yl)-acetamidine with acetic acid (162) (1.7 g, 62.5%) as an off-white solid.

1. filtrationThe reaction mixture was filtered through celite
2. washwashed with 10% methanol in dichloromethane (5×100 mL)
3. customdried
4. concentrationconcentrated
5. washThe yellow solid was washed with 10% ethyl acetate in hexane (3×30 mL)