反应详情

To a solution of compound 5x (0.35 g, 1 mmol, obtained from the above Synthesis Example 12) in dry DMF (20 mL) was added NaH (60% in oil, 2.64 g, 66.0 mmol) at 0° C. for 1 hr. After stirring at room temperature for 8 hrs, epichlorohydrin (0.92 g, 10 mmol) was added and stirred for a further 1 hr. The reaction mixture was partitioned between H2O and CH2Cl2. The organic layer was dried over MgSO4 and concentrated. The resultant residue was purified by column chromatography (MeOH/CH2Cl2=1:10) to give the title compound 5kkk (0.33 g, 84% yield).

1. stirringstirred for a further 1 hr
2. customThe reaction mixture was partitioned between H2O and CH2Cl2
3. dry with materialThe organic layer was dried over MgSO4
4. concentrationconcentrated
5. customThe resultant residue was purified by column chromatography (MeOH/CH2Cl2=1:10)