反应详情

The compound (133 mg, 0.298 mmol) obtained in Example 1a and the compound (132 mg, 0.298 mmol) obtained in Example 93b were dissolved in n-butanol (3 mL), triethylamine (62 μL, 0.447 mmol) was added, and the mixture was stirred with heating to reflux for 15 hours. A solution of the compound (133 mg, 0.298 mmol) obtained in Example 1a in n-butanol (2 mL) was added to the reaction mixture, and the mixture was further stirred with heating to reflux for 24 hours. Subsequently, triethylamine (62 μL, 0.447 mmol) was added to the reaction mixture, and the mixture was further stirred with heating to reflux for 24 hours. The solvent was evaporated under reduced pressure, and the resulting residue was purified by NH silica gel column chromatography (ethyl acetate:methanol=100:0→50:1, v/v) to give the title compound (157 mg; yield, 64%) as a light yellow solid.

1. temperaturewith heating
2. temperatureto reflux for 15 hours
3. stirringthe mixture was further stirred
4. temperaturewith heating
5. temperatureto reflux for 24 hours
6. stirringthe mixture was further stirred
7. temperaturewith heating
8. temperatureto reflux for 24 hours
9. customThe solvent was evaporated under reduced pressure
10. customthe resulting residue was purified by NH silica gel column chromatography (ethyl acetate:methanol=100:0→50:1, v/v)