反应详情

To the compound (0.84 g, 1.86 mmol) obtained in Example 9, Step (i) was added trifluoroacetic acid (12 ml), and the mixture was stirred at room temperature for 20 minutes. Trifluoroacetic acid was evaporated by an evaporator, and DMF (15 ml), 4-(chloromethyl)benzyl alcohol (0.32 g, 2.04 mmol), and potassium carbonate (1.28 g, 9.30 mmol) were added thereto, and the mixture was stirred at room temperature for 18 hours. The carbonate was removed by filtration, and the filtrate was concentrated. Water was added to the residue, and the mixture was extracted three times with chloroform/ethanol=3/1. The resultant was dried over magnesium sulfate, concentrated, and purified by silica gel column (chloroform/methanol=20/1) to give the subtitle compound (0.52 g, 1.11 mmol) as a white solid. Yield: 60%.

1. additionwere added
2. stirringthe mixture was stirred at room temperature for 18 hours
3. customThe carbonate was removed by filtration
4. concentrationthe filtrate was concentrated
5. additionWater was added to the residue
6. extractionthe mixture was extracted three times with chloroform/ethanol=3/1
7. dry with materialThe resultant was dried over magnesium sulfate
8. concentrationconcentrated
9. custompurified by silica gel column (chloroform/methanol=20/1)