反应详情

Ammonium chloride (38 g) was added to a solution of 4-bromo-2-(tert-butyl)-6-nitrophenyl methyl ether (20.6 g) in methanol-water (140 ml-140 ml) and iron (20 g) was gradually added while heating to reflux. The mixture was heated to reflux for 2 hours and then the reaction mixture was filtered through celite. The filtrate was concentrated under reduced pressure, ethyl acetate was added to the residue and the mixture was washed 3 times with brine. The organic layer was dried over anhydrous magnesium sulfate and the solvent was distilled off under reduced pressure to yield a crude product of the title compound (16.65 g) as a brown oil.

1. additionwas gradually added
2. temperaturewhile heating to reflux
3. temperatureThe mixture was heated
4. temperatureto reflux for 2 hours
5. filtrationthe reaction mixture was filtered through celite
6. concentrationThe filtrate was concentrated under reduced pressure, ethyl acetate
7. additionwas added to the residue
8. washthe mixture was washed 3 times with brine
9. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
10. distillationthe solvent was distilled off under reduced pressure