反应详情

温度

50 °C

A mixture of 44 (5.3 g, 18 mmol) in methanolic HCl (200 mL) was heated in an oil bath (50° C., 1 h). The resulting mixture was cooled, diluted with water (50 mL), and stirred at room temperature (30 min). The solvent volume was reduced in vacuo and neutralized with sodium carbonate. The aqueous layer was extracted with three portions of dichloromethane. The combined organic extracts were washed with brine and dried over Na2SO4. The solvent was removed in vacuo. PCTLC (SiO2, 6 mm, 10% EtOH-90% CHCl3) afforded the title compound (45).

1. temperatureThe resulting mixture was cooled
2. extractionThe aqueous layer was extracted with three portions of dichloromethane
3. washThe combined organic extracts were washed with brine
4. dry with materialdried over Na2SO4
5. customThe solvent was removed in vacuo