反应详情

To a solution of 4-chloro-3-nitrobenzoic acid methyl ester (4.00 g, 18 mmol) and 4-mercaptophenol (2.37 g, 18 mmol) in acetone (60 mL) was added Cs2CO3 (5.93 g, 18 mmol) at room temperature, and then the mixture was refluxed for 30 minutes. After cooling to room temperature, the mixture was filtered and the filtrate was evaporated. The residue was diluted with AcOEt (30 mL), washed with H2O (3 times) and brine, dried over MgSO4, and evaporated to give brown oil. The oily residue was separated by silica gel column chromatography (n-hexane/AcOEt=4/3) to give the title compound as yellow amorphous (5.60 g).

1. temperaturethe mixture was refluxed for 30 minutes
2. filtrationthe mixture was filtered
3. customthe filtrate was evaporated
4. additionThe residue was diluted with AcOEt (30 mL)
5. washwashed with H2O (3 times) and brine
6. dry with materialdried over MgSO4
7. customevaporated
8. customto give brown oil
9. customThe oily residue was separated by silica gel column chromatography (n-hexane/AcOEt=4/3)