反应详情

4-Fluoro-3-nitro-5-trifluoromethyl benzoic acid (1.00 g, 4.0 mmol), 2-aminophenol (0.47 g, 4.4 mmol), CHCl3 (20 mL), and WSC (0.83 g, 4.4 mmol) were added together and stirred at room temperature for 1 hour. Water was added, and this was extracted with chloroform/acetone (3:1). After the organic layer obtained was dried over anhydrous sodium sulfate, it was filtered and concentrated. To a dioxane (20 mL) solution of the solid obtained was added methanesulfonic acid (2.28 g, 24 mmol), and this was heated to reflux for 18 hours. After the reaction solution was cooled, water was added, and the precipitated crystals were filtered, and after being washed with water were dried to yield the title compound (0.70 g, 54% yield) as yellowish-brown crystals.

1. extractionthis was extracted with chloroform/acetone (3:1)
2. customAfter the organic layer obtained
3. dry with materialwas dried over anhydrous sodium sulfate, it
4. filtrationwas filtered
5. concentrationconcentrated
6. customTo a dioxane (20 mL) solution of the solid obtained
7. temperaturethis was heated
8. temperatureto reflux for 18 hours
9. temperatureAfter the reaction solution was cooled
10. filtrationthe precipitated crystals were filtered
11. washafter being washed with water
12. customwere dried