反应详情

A mixture of 1.4 g (0.035 mole) of 60% sodium hydride, 25 mL of dioxane, 2.68 g (0.01 mole) of (2-amino-4,5-difluorophenyl)-(2-chlorophenyl)-methanone (Xmm) and 2.23 g (0.016 mole) of 4-morpholinepropanol was stirred at room temperature for 4 hours. The mixture was quenched by the addition of 50 mL of water. The mixture was extracted with ethyl acetate, and the extract washed with water, dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure. The residue was triturated with hexane and then recrystallized from hexane-ethyl acetate to give 2.55 g of (2-amino-5-fluoro-4-(3-(4-morpholinyl)propoxy)phenyl)-(2-chlorophenyl)-methanone (Xi). MH+/Z=393.

1. customThe mixture was quenched by the addition of 50 mL of water
2. extractionThe mixture was extracted with ethyl acetate
3. washthe extract washed with water
4. dry with materialdried over anhydrous sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customThe residue was triturated with hexane
8. customrecrystallized from hexane-ethyl acetate