反应详情

To a stirred solution of 8.0 g (0.042 mole) of 2-chloro-4-fluoro-5-nitrophenol in 200 mL of acetone was added 6.09 g (0.0435 mole) of potassium carbonate. The mixture was heated at reflux temperature for 15 minutes, and 8.9 g (0.063 mole) of iodomethane was added. The resultant mixture was heated at reflux temperature for 5 hours, then stirred at room temperature for approximately 18 hours. The mixture was filtered and the filtrate evaporated under reduced pressure to leave a residue. The residue was dissolved in diethyl ether, filtered, and the filtrate washed with a saturated sodium chloride solution. The ether solution was dried over anhydrous sodium sulfate, filtered, and the filtrate evaporated to yield 6.6 g of 1-chloro-5-fluoro-2-methoxy-4-nitrobenzene as a solid, 63°-65° C.

1. temperatureThe mixture was heated
2. temperatureat reflux temperature for 15 minutes
3. temperatureat reflux temperature for 5 hours
4. filtrationThe mixture was filtered
5. customthe filtrate evaporated under reduced pressure
6. customto leave a residue
7. filtrationfiltered
8. washthe filtrate washed with a saturated sodium chloride solution
9. dry with materialThe ether solution was dried over anhydrous sodium sulfate
10. filtrationfiltered
11. customthe filtrate evaporated