反应详情

温度

20 °C

The product of Example 1, 1, 1-bismethylthio-4,4,4-trifluoro-1-buten-3-one, (4.32 g, 0.02 mol) and the product of Example 4, 6-chloro-3pyridylmethylamine (2.85 g, 0.02 mol) were dissolved in ethanol (50 ml). The resulting solution was heated under reflux for 2 hours under an atmosphere of nitrogen. The resulting mixture was cooled to ambient temperature (20° C.) and the solvent removed by evaporation under reduced pressure. The residue was chromatographically purified using a silica gel column eluted with dichloromethane/ether (19:1) to give the product, 1-(6-chloro-3- pyridylmethyl) amino-1-methylthio-4,4,4-trifluoro-1-buten-3-one, as a solid which recrystallized from ethanol, in a yield of 3.32 g (53%), melting point 112° C.

1. temperatureThe resulting solution was heated
2. temperatureunder reflux for 2 hours under an atmosphere of nitrogen
3. customthe solvent removed by evaporation under reduced pressure
4. customThe residue was chromatographically purified
5. washeluted with dichloromethane/ether (19:1)