反应详情

温度

70 °C

To a solution of 4-[3-(6-bromo-hexyl)-2-(2-ethoxycarbonyl-ethyl)-phenoxy]-butyric acid ethyl ester (3.48 g, 7.4 mmol), 3-bromo-5-hydroxy-N,N-dimethyl-benzamide (1.5 g, 6.17 mmol) in N,N-dimethylformamide (30 mL) and acetone (60 mL) was added potassium carbonate (8.51 g, 61.7 mmol). The resulting suspension was heated to 70° C. for 24 h. Then the reaction mixture was cooled to room temperature and diluted with water and 10% aq. HCl. The organic compound was extracted into ethyl acetate and the combined organic extracts were washed with water and brine solution. The organic extracts were dried over anhydrous sodium sulfate and removal of the solvent under reduced pressure gave the crude product which was purified on ISCO™ column (120 g) using 50% ethyl acetate in hexanes as eluting solvent to give the title compound (3.1 g, 80%) as colorless oil.

1. temperatureThen the reaction mixture was cooled to room temperature
2. extractionThe organic compound was extracted into ethyl acetate
3. washthe combined organic extracts were washed with water and brine solution
4. dry with materialThe organic extracts were dried over anhydrous sodium sulfate and removal of the solvent under reduced pressure
5. customgave the crude product which
6. customwas purified on ISCO™ column (120 g)
7. washas eluting solvent