反应详情

温度

75 °C

To a solution of 3-bromo-5-methanesulfonyl-phenol (1.3 g) in a mixture of acetone and DMF (2:1, 60 mL) were added potassium carbonate (7.1 g) and 4-[3-(6-bromo-hexyl)-2-(2-ethoxycarbonyl-ethyl)-phenoxy]-butyric acid ethyl ester (2.7 g). The resulting mixture was stirred at 75° C. for 1 day. Then the insoluble material was filtered out and the filtrate was diluted with ethyl acetate and washed with water and brine. The organic extract was dried over anhydrous sodium sulfate, concentrated and purified on a silica gel column using ethyl acetate and hexanes to yield the title compound (2.9 g, 87% yield). LRMS calcd for C30H41O8BrS [M+H]+ 641.2, observed 641.1.

1. filtrationThen the insoluble material was filtered out
2. additionthe filtrate was diluted with ethyl acetate
3. washwashed with water and brine
4. extractionThe organic extract
5. dry with materialwas dried over anhydrous sodium sulfate
6. concentrationconcentrated
7. custompurified on a silica gel column