反应详情

温度

70 °C

3′-Hydroxyacetophenone (200 mg) was dissolved in acetonitrile (4 ml). After adding ethyl iodide (0.2 ml) and potassium carbonate (347 mg), the mixture was stirred at 70° C. for 9 hours. After 9 hours, water and ethyl acetate were added to the reaction mixture followed by separation. The organic layer was washed with a saturated aqueous solution of sodium chloride, dried over sodium sulfate, filtered and concentrated. The crude product thus obtained was purified by silica gel chromatography (n-hexane:ethyl acetate=8:1) to thereby give 204 mg of 3′-ethoxyacetophenone. The procedure employed for the synthesis of F-12 was repeated but replacing the 3′-methoxyacetophenone by 3′-ethoxyacetophenone to thereby give (±)-N-(1-(3-ethoxyphenyl)ethyl)-2-(2′,5′-dichlorophenylthio)ethylamine (F-63). MS m/z: 369 (M+).

1. waitAfter 9 hours
2. customfollowed by separation
3. washThe organic layer was washed with a saturated aqueous solution of sodium chloride
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated
7. customThe crude product thus obtained
8. customwas purified by silica gel chromatography (n-hexane:ethyl acetate=8:1)