反应详情

温度

100 °C

To a mixture of (S)-2-[4-(3-bromo-2-fluoro-phenoxy)-2-oxo-2,5-dihydro-pyrrol-1-yl]-4-methyl-pentanoic acid ethyl ester (prepared as in Example 128, 0.850 g, 2.05 mmol), palladium(II) acetate (0.050 g, 0.22 mmol), 2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (0.250 g, 0.40 mmol), and cesium carbonate (1.90 g, 5.83 mmol) in 1,4-dioxane (5 mL) was added a dimethylamine solution in tetrahydrofuran (2M, 3 mL, 6.00 mmol) and the resulting mixture was sealed in a tube and heated at 100° C. for 6 h. The cooled solution was poured into ethyl acetate (100 mL), filtered and the filtrate washed with water, brine and dried over anhydrous sodium sulfate. The resulting mixture was filtered, evaporated and the residue purified by ISCO flash chromatography (Teledyne Isco RediSep Flash Column 40 g, 10% to 60% ethyl acetate/hexanes) which afforded (S)-2-[4-(3-dimethylamino-2-fluoro-phenoxy)-2-oxo-2,5-dihydro-pyrrol-1-yl]-4-methyl-pentanoic acid ethyl ester (0.261 g, 34%) as a yellow oil.

1. customthe resulting mixture was sealed in a tube
2. filtrationfiltered
3. washthe filtrate washed with water, brine
4. dry with materialdried over anhydrous sodium sulfate
5. filtrationThe resulting mixture was filtered
6. customevaporated
7. customthe residue purified by ISCO flash chromatography (Teledyne Isco RediSep Flash Column 40 g, 10% to 60% ethyl acetate/hexanes) which