反应详情

温度

30 °C

To a solution of compound 18 (7.10 g, 25.2 mmol) in 710 mL of anhydrous THF was added EDCI (14.5 g, 75.6 mmol). The resulting suspension was left stirring at 30° C. overnight. The precipitate was filtered and thoroughly washed with DCM. The filtrate was concentrated to dryness and the residue was dissolved in DCM (100 mL). The solution was washed with water (50 mL×2) and brine (50 mL×1). The DCM layer was then dried over anhydrous Na2SO4 and concentrated to give the crude product, which was purified via column chromatography on silica gel (Petroleum ether/EtOAc 200:1→100:1→50:1) to give compound 19 as a white solid. 1H NMR (CDCl3; 400 MHz) δ 7.36 (s), δ 7.10 (s), δ 1.53 (s), δ 1.41 (s).

1. waitThe resulting suspension was left
2. filtrationThe precipitate was filtered
3. washthoroughly washed with DCM
4. concentrationThe filtrate was concentrated to dryness
5. dissolutionthe residue was dissolved in DCM (100 mL)
6. washThe solution was washed with water (50 mL×2) and brine (50 mL×1)
7. dry with materialThe DCM layer was then dried over anhydrous Na2SO4
8. concentrationconcentrated
9. customto give the crude product, which
10. customwas purified via column chromatography on silica gel (Petroleum ether/EtOAc 200:1→100:1→50:1)