反应详情

Add methanesulfonyl chloride (0.035 mL, 0.45 mmol) to a solution of 5-phenylethynyl-pyridin-3-ylamine dihydrochloride, (prepared as described in EXAMPLE 155), (0.120 g, 0.45 mmol) and pyridine (0.075 mL, 0.90 mmol) in dichloromethane (2.5 mL) at 0° C. Warm to room temperature and stir overnight. Add pyridine (0.020 mL, 0.24 mmol) and methanesulfonyl chloride (0.010 mL, 0.11 mmol), stir for 20 h and add water. Separate the layers and concentrate the organic phase. Purify by silica gel chromatography, eluting with 1.1 hexanes:ethyl acetate, to give the title compound (0.091 g, 75%).

1. customSeparate the layers
2. concentrationconcentrate the organic phase
3. customPurify by silica gel chromatography
4. washeluting with 1.1 hexanes