反应详情

3-[4-(5,6-dimethoxy-3-methyl-1,4-benzoquinon-2-ylmethyl)phenyl]propionic acid diazomethyl ketone (70 mg, 0.20 mmol) obtained in Step 1 of Method B of Production Example 26 was dissolved in dry ethanol (5 ml), to which were added silver nitrate (34 mg, 0.20 mmol) and morpholine (0.090 ml, 1.0 mmol), and the mixture was heated to reflux for 20 minutes. The reaction mixture was filtered and the solid was washed with ethanol. The filtrate and the wash solution were combined and the solvent was distilled off, the resulting residue was purified by a silica gel column chromatography (hexane:ethyl acetate=1:3) to yield the title compound (42 mg, 0.098 mmol, yield 49%).

1. temperaturethe mixture was heated
2. temperatureto reflux for 20 minutes
3. filtrationThe reaction mixture was filtered
4. washthe solid was washed with ethanol
5. distillationthe solvent was distilled off
6. customthe resulting residue was purified by a silica gel column chromatography (hexane:ethyl acetate=1:3)