反应详情

4-cyano-2-fluorobenzoic acid (1.20 g), HOBt (1.47 g), WSC•monohydrochloride (2.10 g) and DMF (20 ml) were mixed with one another and stirred for 30 minutes. 2M methylamine-THF solution (11 ml) was added thereto, followed by stirring for 30 minutes. Water was added to the reaction solution, followed by extraction with ethyl acetate. The organic layer was washed with water and then saturated brine in this order, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography (chloroform:methanol=100:1). The resulting solid was washed with n-hexane, to obtain 4-cyano-2-fluoro-N-methylbenzamide (1.03 g) as a white solid.

1. stirringby stirring for 30 minutes
2. extractionfollowed by extraction with ethyl acetate
3. washThe organic layer was washed with water
4. dry with materialsaturated brine in this order, and dried over anhydrous magnesium sulfate
5. customthe solvent was evaporated under reduced pressure
6. customThe resulting residue was purified by silica gel column chromatography (chloroform:methanol=100:1)
7. washThe resulting solid was washed with n-hexane