反应详情

温度

120 °C

To a solution of 4-hydroxy-6-methyl-2-oxo-1,2-dihydropyridine (3-2; 20.1 g; 161 mmol) in NMP (1.6 L) was added 3-chloro-5-fluorobenzonitrile (3-1; 25 g; 161 mmol) and potassium carbonate (44.4 g; 321 mmol). The resulting solution stirred at 120° C. overnight. The reaction mixture was cooled to ambient temperature and diluted with 4 L of ice-water. The aqueous layer was acidified to pH 5 to precipitate out the product. The precipitate was collected via filtration, washed with water, and air dried. The crude solid product was triturated in 5% methanol/dichloromethane and filtered to give a solid. The solid was triturated with 1:1 ethyl acetate:hexane, stirred, and filtered to afford the title product as a tan solid. MS M+1=261.0.

1. temperatureThe reaction mixture was cooled to ambient temperature
2. customto precipitate out the product
3. filtrationThe precipitate was collected via filtration
4. washwashed with water, and air
5. customdried
6. customThe crude solid product was triturated in 5% methanol/dichloromethane
7. filtrationfiltered
8. customto give a solid
9. customThe solid was triturated with 1:1 ethyl acetate
10. stirringhexane, stirred
11. filtrationfiltered