反应详情

To a solution of 18 (1.8 g, 8.71 mmol) in acetone (80 mL) were added 4-(2-chloroethyl)morpholine hydrochloride (1.95 g, 10.5 mmol), potassium iodide (360 mg, 2.2 mmol) and potassium carbonate (6.0 g, 44.0 mmol), respectively. The reaction mixture was refluxed for 16 h and concentrated. The residue was diluted with water and the aqueous phase was extracted twice with EtOAc. The combined organic extracts were dried over anhydrous Na2SO4, filtered and concentrated to form a residue was purified by flash chromatography on silica gel (EtOAc/CH2Cl2, 50/50 to MeOH/CH2Cl2: 2/98) to afford the title compound 19 (2.7 g, 8.4 mmol, 96% yield).

1. temperatureThe reaction mixture was refluxed for 16 h
2. concentrationconcentrated
3. additionThe residue was diluted with water
4. extractionthe aqueous phase was extracted twice with EtOAc
5. dry with materialThe combined organic extracts were dried over anhydrous Na2SO4
6. filtrationfiltered
7. concentrationconcentrated
8. customto form a residue
9. customwas purified by flash chromatography on silica gel (EtOAc/CH2Cl2, 50/50 to MeOH/CH2Cl2: 2/98)