反应详情

Add a solution of isobutynyl chloride (0.09 g, 1.08 mmol) dissolved in tetrahydrofuran to a solution of 5-(3-amino-4-fluorophenylethynyl) -nicotinonitrile, (prepared as described in EXAMPLE 160), (0.2 g, 0.8 mmol) in anhydrous tetrahydrofuran and stir overnight at room temperature. Pour into ethyl acetate, wash with water and an aqueous saturated solution of sodium chloride, dry (potassium carbonate), filter and concentrate. Purify the residue by silica gel chromatography, eluting with 100:0 to 95:5 dichloromethane:ethyl acetate, to give the title compound as a white solid (210 mg, 84%).

1. washwash with water
2. dry with materialan aqueous saturated solution of sodium chloride, dry (potassium carbonate)
3. filtrationfilter
4. concentrationconcentrate
5. customPurify the residue by silica gel chromatography
6. washeluting with 100:0 to 95:5 dichloromethane