反应详情

A solution of 2-Chloro-5-nitroaniline (3 g, 17.4 mmole), 4-hydroxythiophenol (2.4 g, 19.0 mmol), cesium carbonate (12.35 g, 38 mmol) in dimethylformamide (35 ml) was heated at 100° C. for 16 hours. Afterwards ice water (200 mL) was added to the solution and to the resultant slurry was added ethyl acetate (200 ml). The layers were separated and the organic layer was washed with 10% sodium bicarbonate and 10% sodium chloride, dried over anhydrous sodium sulfate. The drying agent was filtered and solvent was removed under vacuum leaving a yellow oil. The oil was purified by silica gel chromatography eluting with methylene chloride/methanol (97:3), to provide a yellow solid (4-(2-Amino-4-nitro-phenylsulfanyl)-phenol) (2.1g, 46%).

1. customThe layers were separated
2. washthe organic layer was washed with 10% sodium bicarbonate and 10% sodium chloride
3. dry with materialdried over anhydrous sodium sulfate
4. filtrationThe drying agent was filtered
5. customsolvent was removed under vacuum
6. customleaving a yellow oil
7. customThe oil was purified by silica gel chromatography
8. washeluting with methylene chloride/methanol (97:3)