反应详情

To a solution of 1-bromo-3,5-dinitrobenzene (20 g, 80.97 mmol) in acetic acid (120 ml) at 90° C. was added iron powder (11.3 g, 202.4 mmol, 2.5 eq) slowly portionwise over a period of 30 min (caution: highly exothermic reaction). After completion of the addition, the mixture was quenched by the addition of crushed ice. The precipitate formed was filtered and was washed with cold water to obtain orange solid. The solid was dried under vacuum to give the product in 80% yield (14 g). 1H NMR (300 MHz, CDCl3): δ 10.55 (br s, 2H), 8.46 (s, 1H), 8.19 (s, 1H), 8.02 (s, 1H).

1. customhighly exothermic reaction)
2. additionAfter completion of the addition
3. customthe mixture was quenched by the addition of crushed ice
4. customThe precipitate formed
5. filtrationwas filtered
6. washwas washed with cold water
7. customto obtain orange solid
8. customThe solid was dried under vacuum
9. customto give the product in 80% yield (14 g)