反应详情

An argon filled Schlenk flask was charged with 25.77 g (104 mmol) of 2-bromo-1,3-dinitrobenzene, 150 mL of absolute methanol was added and the reaction mixture was chilled in an ice bath. 2.4 g (104 mmol) of Na was added, and the resulting reaction mixture was purged with argon until all Na was dissolved and stirred at RT over night. The solvent was removed, the residue was re-suspended in acetone and filtered through Celite to remove NaBr. The solvent was removed, and the crude product was recrystallized from iPrOH. Yield: 19.8 g (90%). 1H NMR (CDCl3): δ 8.05 (d, JHH=8.2 Hz, 2H, Ar), 7.38 (t, JHH=8.2 Hz, 1H, Ar), 4.07 (s, 3H, OCH3) ppm.

1. additionwas added
2. temperaturethe reaction mixture was chilled in an ice bath
3. customthe resulting reaction mixture
4. customwas purged with argon until all Na
5. dissolutionwas dissolved
6. customThe solvent was removed
7. filtrationfiltered through Celite
8. customto remove NaBr
9. customThe solvent was removed
10. customthe crude product was recrystallized from iPrOH