反应详情

温度

25 °C

To a stirred solution of 2,6-Dibromo-3,5-dihydroxy-4[(dimethylamino) methylene]-benzoic Acid (1 mmol) in 2.5 mL of 3 N NaOH under nitrogen was added 0.345 g of Raney nickel in portions over a period of 1 h. The mixture was then stirred at 25° C. for about 12 h and filtered. The filter cake was washed with water (2×5 mL), and the combined filtrates were acidified to a pH of 1 with concentrated HCl to give a pale yellow or light purple solution. The solution was extracted with ethyl acetate, and the combined organic extracts were washed with saturated NaCl solution (2×0.2 mL), dried over sodium sulphate and evaporated by a rotatory evaporator to give 3,5-Dihydroxy-4-methylbenzoic Acid (70%) as a white solid: 1H NMR (DMSO-d6) δ 6.90 (s, 2H), 1.95 (s, 3H).

1. filtrationfiltered
2. washThe filter cake was washed with water (2×5 mL)
3. customto give a pale yellow or light purple solution
4. extractionThe solution was extracted with ethyl acetate
5. washthe combined organic extracts were washed with saturated NaCl solution (2×0.2 mL)
6. dry with materialdried over sodium sulphate
7. customevaporated by a rotatory evaporator