反应详情

温度

60 °C

A mixture of the compound (0.47 g) obtained in Example (54h) and 1N NaOH (3 ml) in methan61 (3 ml) was heated for 30 minutes under reflux. The reaction mixture was adjusted to pH 3-4 with 1N HCl. Resulting crystalline precipitates were collected by filtration and recrystallized from ethyl acetate--hexane. The crystals were suspended in water (2 ml), and the suspension was stirred for 2 hours at 60° C. Insoluble materials were collected by filtration and dried to afford colorless crystals (0.25 g, 54%). This product was in agreement with that obtained in Example 1.

1. temperaturewas heated for 30 minutes
2. temperatureunder reflux
3. customResulting crystalline precipitates
4. filtrationwere collected by filtration
5. customrecrystallized from ethyl acetate
6. filtrationInsoluble materials were collected by filtration
7. customdried