反应详情

Methyl iodide (6.5 mL, 104 mmol) and potassium hydrogencarbonate (17.0 g, 170 mmol) were added to a DMF (200 mL) solution of the compound obtained in Example 21 (26.1 g, 85 mmol), and the mixture was stirred at room temperature overnight. The solvents were distilled off under a reduced pressure, water was added to the residue, and the product was extracted with ethyl acetate. The organic layer was washed with a saturated sodium chloride solution and then dried over anhydrous sodium sulfate, and the solvents were distilled off under a reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=5:1), to give 24.0 g (88%) of the captioned compound.

1. distillationThe solvents were distilled off under a reduced pressure, water
2. additionwas added to the residue
3. extractionthe product was extracted with ethyl acetate
4. washThe organic layer was washed with a saturated sodium chloride solution
5. dry with materialdried over anhydrous sodium sulfate
6. distillationthe solvents were distilled off under a reduced pressure
7. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=5:1)