反应详情

温度

25 °C

10,11-Dimethoxy-5,6,8,12b-tetrahydro-isoindolo-[1,2-a]isoquinoline (109.65 g) and potassium hydroxide in pellet form (23.2 g) are dissolved in methanol (1100 cc). Air is bubbled into the reaction mixture, which is heated under reflux for 3 hours and then maintained at 25° C. for 48 hours. After concentration to 500 cc, the addition of distilled water (5000 cc) and stirring for 2 hours, a precipitate appears which is filtered off, washed three times with distilled water (total 500 cc) and dried under reduced pressure (20 mm Hg) at 40° C. A crude product (104.65 g), melting at 219° C., is obtained. A solution of a portion of this product (30 g) in dimethylformamide (200 cc) at 120° C. is treated with decolourising charcoal (1 g), filtered whilst hot, and cooled at about 5° C. for 16 hours. The resulting crystals are filtered off, washed three times with diisopropyl ether (total 30 cc) and dried under reduced pressure (1 mm Hg) at 60° C. for 6 hours. 12b-Hydroxy-10,11-dimethoxy-5,6,8,12b-tetrahydro-isoindolo[1,2-a]isoquinol-8-one (16.70 g), melting at 220° C., is thus obtained.

1. customAir is bubbled into the reaction mixture, which
2. temperatureis heated
3. temperatureunder reflux for 3 hours
4. concentrationAfter concentration to 500 cc
5. additionthe addition of distilled water (5000 cc)
6. filtrationis filtered off
7. washwashed three times with distilled water (total 500 cc)
8. customdried under reduced pressure (20 mm Hg) at 40° C
9. customA crude product (104.65 g), melting at 219° C., is obtained
10. filtrationfiltered whilst hot, and
11. temperaturecooled at about 5° C. for 16 hours
12. filtrationThe resulting crystals are filtered off
13. washwashed three times with diisopropyl ether (total 30 cc)
14. customdried under reduced pressure (1 mm Hg) at 60° C. for 6 hours