反应详情

温度

60 °C

To 8.0 g of 2,8-diacetylamino-6-fluoro-5-methyl-1 -tetralone, 120 ml of a 20% aqueous solution of hydrochloric acid were added and the mixture was stirred at an external temperature of 60° C. for 2 hours. After the completion of the reaction, the reaction mixture was cooled and was added with 100 ml of water. The resulting mixture was filtered through a Kiriyama funnel. To the filtrate, further 100 ml of water were added, followed by extraction with chloroform. To the chloroform layer so obtained, potassium carbonate and Florisil were added and they were stirred for a while. The resulting mixture was filtered and then, the solvent was removed under reduced pressure. The residue so obtained was recrystallized from chloroform-diethyl ether, whereby 3.4 g of the title compound was obtained.

1. customAfter the completion of the reaction
2. temperaturethe reaction mixture was cooled
3. filtrationThe resulting mixture was filtered through a Kiriyama funnel
4. additionTo the filtrate, further 100 ml of water were added
5. extractionfollowed by extraction with chloroform
6. customTo the chloroform layer so obtained
7. stirringthey were stirred for a while
8. filtrationThe resulting mixture was filtered
9. customthe solvent was removed under reduced pressure
10. customThe residue so obtained
11. customwas recrystallized from chloroform-diethyl ether