反应详情

温度

35 °C

To a solution of magnesium (2.23 g) and iodine (5 mg) in diethyl ether (20 mL) was added dropwise a solution of 1-bromo-3,4-dichlorobenzene (20.7 g) in diethyl ether (20 ml), and the mixture was stirred at 35° C. for 1 hr. The reaction mixture was cooled to −10° C., and diethyl ether (100 mL) was added. A solution of (4-methoxyphenoxy)acetonitrile (10 g) in diethyl ether (20 ml) was added dropwise at −10° C., and the mixture was stirred for 1 hr while warming to room temperature. To the reaction mixture was added 1 N aqueous HCl solution (200 ml), and the mixture was stirred at room temperature for 1 hr, and extracted with ethyl acetate. The obtained extract was washed with water and brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography (NH, ethyl acetate/hexane) to give the title compound (15.6 g).

1. temperatureThe reaction mixture was cooled to −10° C.
2. stirringthe mixture was stirred for 1 hr
3. temperaturewhile warming to room temperature
4. stirringthe mixture was stirred at room temperature for 1 hr
5. extractionextracted with ethyl acetate
6. extractionThe obtained extract
7. washwas washed with water and brine
8. dry with materialdried over anhydrous magnesium sulfate
9. customThe solvent was evaporated under reduced pressure
10. customThe obtained residue was purified by silica gel column chromatography (NH, ethyl acetate/hexane)