反应详情

Compound 32 (391 mg, 1.00 mmol) was dissolved in 1,4-dioxane (10 mL), and morpholine (0.44 mL, 5.00 mmol) was added thereto, followed by stirring under heating and reflux for 10 hours. The reaction mixture was concentrated under reduced pressure, and a saturated aqueous solution of sodium chloride was added to the resulting residue, followed by extraction with chloroform. The organic layer was washed with a saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate, and then the solvent was distilled away under reduced pressure. The resulting residue was purified through silica gel column chromatography (chloroform:methanol=19:1) to afford the entitled Compound 34 (372 mg, 84%).

1. temperatureunder heating
2. temperaturereflux for 10 hours
3. concentrationThe reaction mixture was concentrated under reduced pressure
4. additiona saturated aqueous solution of sodium chloride was added to the resulting residue
5. extractionfollowed by extraction with chloroform
6. washThe organic layer was washed with a saturated aqueous solution of sodium chloride
7. dry with materialdried over anhydrous magnesium sulfate
8. distillationthe solvent was distilled away under reduced pressure
9. customThe resulting residue was purified through silica gel column chromatography (chloroform:methanol=19:1)