反应详情

温度

50 °C

The product of Example 1, 1,1-bismethylthio-4,4,4-trifluoro-1-buten-2-one, (2.16 g, 0.01 mol) and dimethylamine (0.45 g, 0.01 mol) were dissolved in ethanol (30 ml). The resulting solution was heated to 50° C. and maintained at that temperature with stirring for 1 hour. After this time, the resulting mixture was cooled to ambient temperature (20° C.) and the solvent was removed by evaporation under reduced pressure yielding a yellow residue. Chromatographic purifications of the solid using a silica column eluted with dichloromethane/methanol (30:1) gave the product, 1-dimethylamino-1-methylthio-4,4,4-trifluoro-1-buten-3-one, as a yellow oil in a yield of 2.1 g (98%).

1. temperaturemaintained at that temperature
2. temperatureAfter this time, the resulting mixture was cooled to ambient temperature (20° C.)
3. customthe solvent was removed by evaporation under reduced pressure
4. customyielding a yellow residue
5. washeluted with dichloromethane/methanol (30:1)