反应详情

Compound 9 (0.291 g) obtained in Example 9 was dissolved in dichloromethane (2.9 ml) and thionyl chloride (1.5 ml) was added thereto, followed by stirring at room temperature for one hour. The solvent was distilled off under reduced pressure, the residue was again dissolved in toluene, and the solvent was distilled off under reduced pressure. Benzyl alcohol (2 ml) was added to the residue followed by heating under reflux for 30 minutes. The reaction solution was concentrated and the residue was recrystallized from ethanol to give Compound 13 (0.3.04 g, 85.2%) as a white solid.

1. distillationThe solvent was distilled off under reduced pressure
2. dissolutionthe residue was again dissolved in toluene
3. distillationthe solvent was distilled off under reduced pressure
4. additionBenzyl alcohol (2 ml) was added to the residue
5. temperatureby heating
6. temperatureunder reflux for 30 minutes
7. concentrationThe reaction solution was concentrated
8. customthe residue was recrystallized from ethanol