反应详情

温度

40 °C

To a mixture of 4-bromo-2-(2-bromophenylsulfanyl)-nitrobenzene, 1e (15.56 g; 40 mmol) in acetic acid (200 mL) and methanol (400 mL) was added zinc (15.7 g; 240 mmol) over a 30 min period. The mixture was heated to 40° C. for 1 h overnight, filtered, evaporated, and dried under vacuum overnight. The residue was suspended in 1N NaOH solution and extracted with methylene chloride. The organic phase was dried over MgSO4, filtered, and evaporated. The residue was purified via flash column chromatography (eluent gradient: 0 to 10% EtOAc in heptane) to yield 14.2 g (99%) of title compound 4-bromo-2-(2-bromophenylsulfanyl)-aniline, 2e.

1. filtrationfiltered
2. customevaporated
3. customdried under vacuum overnight
4. extractionextracted with methylene chloride
5. dry with materialThe organic phase was dried over MgSO4
6. filtrationfiltered
7. customevaporated
8. customThe residue was purified via flash column chromatography (eluent gradient: 0 to 10% EtOAc in heptane)