反应详情

温度

60 °C

1.86 g of an aqueous methylamine solution (40%) was added dropwise to a mixture of 1.71 g of 2-chloro-5-trifluoromethylsulfanylpyridine and 16 ml of NMP, and then the mixture was heated to 60° C. and heated and stirred for 2 hours. After cooling the mixture to room temperature, 1.66 g of potassium carbonate was added, and 1.86 g of a 40% aqueous methylamine solution was added dropwise. The mixture was heated to 60° C. and further heated and stirred for 2 hours. After cooling the mixture to room temperature, water was added, and the mixture was extracted with ethyl acetate. The combined organic layer was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The resulting residue was applied to a silica gel column chromatography to obtain 1.52 g of methyl-(5-trifluoromethylsulfanylpyridin-2-yl)-amine.

1. temperatureheated
2. temperatureAfter cooling the mixture to room temperature
3. temperatureThe mixture was heated to 60° C.
4. temperaturefurther heated
5. stirringstirred for 2 hours
6. temperatureAfter cooling the mixture to room temperature
7. extractionthe mixture was extracted with ethyl acetate
8. dry with materialThe combined organic layer was dried over anhydrous magnesium sulfate
9. concentrationconcentrated under reduced pressure