反应详情

470 mg of the amorphous compound obtained in Example 5 was dissolved in 8 ml of dimethylformamide, and to the solution were sequentially added 30 mg of 60% sodium hydride and 0.1 ml of methyl iodide with ice cooling, and after stirring for two hours with ice cooling was added saturated sodium chloride, and the mixture was extracted with 50 ml of ethyl acetate. The extract was washed with saturated sodium chloride aqueous solution, dried over magnesium sulfate and concentrated under a reduced pressure to obtain a residue, which was then applied to a silica gel column and eluted with hexane/ethyl acetate (1:1) to obtain 413 mg of the title compound in a colorless amorphous form.

1. extractionthe mixture was extracted with 50 ml of ethyl acetate
2. washThe extract was washed with saturated sodium chloride aqueous solution
3. dry with materialdried over magnesium sulfate
4. concentrationconcentrated under a reduced pressure
5. customto obtain a residue, which
6. washeluted with hexane/ethyl acetate (1:1)