反应详情

Add acetic anhydride (113 mg, 1.11 mmol) to a solution of 5-(5-chloropyridin-3-ylethynyl)-2-fluorophenylamine, (prepared as described in EXAMPLE 190) (0.275 g, 1.11 mmol) in pyridine (4 mL). Stir the mixture at room temperature under nitrogen for 18 h then concentrate. Purify by silica gel chromatography, eluting with a gradient of 75:25 to 50:50 with hexanes:ethyl acetate, followed by a second silica gel chromatography, eluting with 75:25 to 60:40 hexanes:ethyl acetate, to give the title compound as a white solid (240 mg, 75%).

1. concentrationthen concentrate
2. customPurify by silica gel chromatography
3. washeluting with a gradient of 75:25 to 50:50 with hexanes
4. washeluting with 75:25 to 60:40 hexanes