反应详情

温度

150 °C

28 g of sodium pentafluoropropionate and 14 g of copper iodide were added to a mixture of 7.2 g of 2-chloro-5-iodopyridine, 75 ml of NMP and 75 ml of xylene under room temperature, and the mixture was heated to 150° C. and heated and stirred for 5.5 hours. After cooling the mixture to 80° C., 180 ml of an aqueous methylamine solution (40%) was added in 4 parts every 2 hours, and the mixture was heated and stirred for 8.5 hours. After the reaction, the mixture was ice-cooled to 0° C, a 28% aqueous ammonia solution and a saturated aqueous sodium bicarbonate solution were added, and the mixture was extracted with methyl tert-butyl ether (hereinafter, referred to as MTBE). The combined organic layer was dried over anhydrous sodium sulfate and then concentrated under reduced pressure. The residue was applied to a silica gel column chromatography to obtain 4.6 g of methyl-(5-pentafluoroethyl-pyridin-2-yl)-amine.

1. temperatureheated
2. temperatureAfter cooling the mixture to 80° C.
3. temperaturethe mixture was heated
4. stirringstirred for 8.5 hours
5. customAfter the reaction
6. temperaturecooled to 0° C
7. extractionthe mixture was extracted with methyl tert-butyl ether (hereinafter,
8. dry with materialThe combined organic layer was dried over anhydrous sodium sulfate
9. concentrationconcentrated under reduced pressure