反应详情

温度

100 °C

3.33 g (13.2 mmol) of 2-acetyl-3-(3-chlorophenyl) acrylic acid ethylester was dissolved in 30 ml of n-butanol. 2.93 g (10.5 mmol) of methylisothiourea-sulfate and 2.00 g (19.8 mmol) of triethylamine were added at room temperature and stirred at 100° C. for one day. After n-butanol was evaporated under reduced pressure, the reaction mixture was diluted with ethyl acetate and washed with saturated aqueous sodium chloride solution. The organic layer was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The residue was purified by the silica gel chromatography (hexane/ethyl acetate=10/1) to obtain the title compound.

1. customAfter n-butanol was evaporated under reduced pressure
2. additionthe reaction mixture was diluted with ethyl acetate
3. washwashed with saturated aqueous sodium chloride solution
4. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
5. concentrationconcentrated under reduced pressure
6. customThe residue was purified by the silica gel chromatography (hexane/ethyl acetate=10/1)