反应详情

To a solution of the title compound of Step B (1.7 g, 5.9 mmol) in methanol (20 mL) was added β-alanine methyl ester hydrochloride (832 mg, 5.9 mmol) followed by sodium methoxide (2.7 mL, 25 wt % in methanol, 11.8 mmol) and the mixture was heated at reflux for 1.5 hour. The mixture was then cooled, stirred overnight at ambient temperature and again heated at reflux for 3 hours. The mixture was then cooled, concentrated and triturated with dichloromethane. The soluble fraction was then purified by flash column chromatography (silica gel, ethyl ether) to give the title compound of Step C as a white solid (0.12 g).

1. temperaturethe mixture was heated
2. temperatureat reflux for 1.5 hour
3. temperatureThe mixture was then cooled
4. temperatureagain heated
5. temperatureat reflux for 3 hours
6. temperatureThe mixture was then cooled
7. concentrationconcentrated
8. customtriturated with dichloromethane
9. customThe soluble fraction was then purified by flash column chromatography (silica gel, ethyl ether)