反应详情

Dissolve 5-(3-amino-4-fluorophenylethynyl)-nicotinonitrile, (prepared as described in EXAMPLE 160), (0.2 g, 0.8 mmol) in anhydrous pyridine. A solution of acetyl chloride (0.07 g, 0.88 mmol) in tetrahydrofuran is added to the reaction and stirred overnight at room temperature. Concentrate and dissolve the crude reaction in ethyl acetate and water. Wash the organic layer with water, an aqueous saturated solution of sodium chloride, dry (potassium carbonate), filter, concentrate and purify (silica gel chromatography, eluting with 95:5 to 80:20 dichloromethane:ethyl acetate), to give the title compound as a white solid (180 mg, 81%).

1. concentrationConcentrate
2. dissolutiondissolve the crude
3. customreaction in ethyl acetate
4. washWash the organic layer with water
5. dry with materialan aqueous saturated solution of sodium chloride, dry (potassium carbonate)
6. filtrationfilter
7. concentrationconcentrate
8. custompurify
9. wash(silica gel chromatography, eluting with 95:5 to 80:20 dichloromethane:ethyl acetate)