反应详情

Acetic anhydride (21 μL) was added to a solution of (2E)-3-(4-tert-butylphenyl)-3-(5-chloro-6-methoxypyridin-2-yl)prop-2-en-1-amine in pyridine (1 mL), and the mixture was stirred at room temperature for 1.5 hours. 1 M hydrochloric acid was added to the reaction solution, followed by extraction with chloroform. The organic layer was dried over magnesium sulfate and filtered, after which the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=3:1→1:1) to give N-[(2E)-3-(4-tert-butylphenyl)-3-(5-chloro-6-methoxypyridin-2-yl)prop-2-en-1-yl]acetamide as a pale yellow amorphous (50 mg, 67% (two steps)).

1. extractionfollowed by extraction with chloroform
2. dry with materialThe organic layer was dried over magnesium sulfate
3. filtrationfiltered
4. customafter which the solvent was evaporated under reduced pressure
5. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=3:1→1:1)