反应详情

温度

80 °C

To a solution of ethyl 6-chloro-5-methylpyrimidine-4-carboxylate (41) (80 g, 398.0 mmol) dissolved in dioxane (800 ml) were added dimethyl amine in THF (2M, 600 ml, 1196.0 mmol) and diisopropyl ethylamine (330 ml, 1990.0 mmol). The reaction mixture was heated to 80° C. for 16 h. Then the mixture is cooled to room temperature, diluted with water, and extracted with EtOAc (2×50 mL). The combined organic layer was washed with water, brine, dried over sodium sulfate, and concentrated at reduced pressure to yield ethyl 6-(dimethylamino)-5-methylpyrimidine-4-carboxylate (45) as a light yellow liquid; yield: 60 g (72%).

1. temperatureThen the mixture is cooled to room temperature
2. extractionextracted with EtOAc (2×50 mL)
3. washThe combined organic layer was washed with water, brine
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated at reduced pressure