反应详情

温度

-15 °C

Cyanuric chloride (7.30 g, 39.6 mmol) was dissolved in toluene (100 ml), cooled to -15° C., added with anhydrous sodium carbonate (4.19 g, 39.6 mmol), stirred for 10 minutes and gradually added dropwise with N-methylaniline (4.24 g, 39.2 mmol) dissolved in toluene (50 ml). This reaction mixture was stirred at the same temperature for 30 minutes and then stirred at room temperature overnight. The reaction mixture was evaporated under reduced pressure. The residue was added with dichloromethane and water, and then shaken for mixing. The organic layer was separated from the mixture, washed with water and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure and the obtained residue was purified by silica gel column chromatography, using n-hexane and ethyl acetate (4: 1) as eluant, to obtain 6.13 g (yield: 60.6%) of 2,4-dichloro-6-(N-methyl-N-phenylamino)-1,3,5-triazine as colorless crystals having melting point of 131.5° C.-132.5° C.

1. stirringThis reaction mixture was stirred at the same temperature for 30 minutes
2. stirringstirred at room temperature overnight
3. customThe reaction mixture was evaporated under reduced pressure
4. additionThe residue was added with dichloromethane and water
5. stirringshaken
6. additionfor mixing
7. customThe organic layer was separated from the mixture
8. washwashed with water
9. dry with materialdried over anhydrous magnesium sulfate
10. customThe solvent was removed under reduced pressure
11. customthe obtained residue was purified by silica gel column chromatography