反应详情

温度

120 °C

7-Amino-4-methyl-3-coumarinylacetic acid (43.1 mg, 0.18 mmol) was dissolved in MeOH (40 ml). H2SO4 (5 drops) was added, and the reaction mixture was heated to 120° C. and stirred. After 4 hr, the disappearance of the starting materials was confirmed, and the reaction mixture was cooled to room temperature. The reaction mixture was concentrated to ⅓ and the mixture was neutralized with aqueous saturated NaHCO3 solution. The reaction mixture was extracted with BuOH, and the organic layer was concentrated. The residue was purified by silica gel column chromatography (eluate: hexane:EtOAc=1:2) to give the object compound (34.4 mg, 0.14 mmol, 75%).

1. temperaturethe reaction mixture was cooled to room temperature
2. concentrationThe reaction mixture was concentrated
3. extractionThe reaction mixture was extracted with BuOH
4. concentrationthe organic layer was concentrated
5. customThe residue was purified by silica gel column chromatography (eluate: hexane:EtOAc=1:2)