反应详情

温度

4 °C

A solution of 4-bromo-2-trifluoromethoxy-benzaldehyde (550 mg, 2.04 mmol) in 1,4-dioxane (27 mL) and H2O (9 mL) was cooled at 4° C. To the solution were added amidosulfuric acid (296 mg, 3.05 mmol) and sodium dihydrogen phosphate dihydrate (1.4 g, 8.98 mmol). The mixture was stirred at 4° C. for 15 min. To the reaction mixture was added a solution of sodium chlorite (238 mg, 2.63 mmol) in H2O (1.5 mL) and stirred at 4° C. for 15 min. To the reaction mixture was added Na2CO3 (304 mg, 2.41 mmol) and stirred at 4° C. for 15 min. The mixture was acidified with conc-HCl (pH=1), and the aqueous layer was extracted with CHCl3 (three times). The combined organic layer was dried over MgSO4, filtered, concentrated, and purified by flash chromatography (silica gel, 1% MeOH in CHCl3) to give 4-bromo-2-trifluoromethoxy-benzoic acid (471 mg, 81%) as a white solid.

1. stirringstirred at 4° C. for 15 min
2. stirringstirred at 4° C. for 15 min
3. extractionthe aqueous layer was extracted with CHCl3 (three times)
4. dry with materialThe combined organic layer was dried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated
7. custompurified by flash chromatography (silica gel, 1% MeOH in CHCl3)