反应详情

Compound 65 (1.0 g) was suspended in methanol (5.0 mL) and maleic acid (307 mg) was added to the suspension at room temperature (20 to 30° C.). After the compound was dissolved, the mixture was concentrated under reduced pressure. Then, isopropanol (5.0 mL) was added to the resulting residue and the mixture was stirred under reflux. Water (0.4 mL) was then added portionwise. Once the residue was dissolved, the mixture was stirred overnight as it was allowed to cool. Subsequently, the mixture was stirred and cooled with ice for 1 hour and was suction-filtered. The resulting solid was washed with isopropanol and dried to give 1.1 g (86% yield) of the desired product as white crystals.

1. dissolutionAfter the compound was dissolved
2. concentrationthe mixture was concentrated under reduced pressure
3. additionThen, isopropanol (5.0 mL) was added to the resulting residue
4. temperatureunder reflux
5. additionWater (0.4 mL) was then added portionwise
6. dissolutionOnce the residue was dissolved
7. stirringthe mixture was stirred overnight as it
8. temperatureto cool
9. stirringSubsequently, the mixture was stirred
10. temperaturecooled with ice for 1 hour
11. filtrationwas suction-filtered
12. washThe resulting solid was washed with isopropanol
13. customdried