反应详情

In 100 ml of THF was dissolved 3.00 g of 3,4-dihydro-9-(3-fluorobenzylamino)acridin-1(2H)-one. The mechanically stirred solution was cooled in ice under nitrogen and 4.68 ml of 1M lithium aluminum hydride in THF was added dropwise over 15 minutes. After 0.5 hour, analysis by TLC indicated the reaction was complete, so it was neutralized with 1 ml of saturated ammonium chloride solution and the resulting salts were filtered. The filtrate was evaporated to an oil which crystallized on trituration with pentane. The solid was filtered and recrystallized from 1:1 dichloromethane/pentane to yield 2.50 g of solid, mp 128° C.

1. temperatureThe mechanically stirred solution was cooled in ice under nitrogen
2. filtrationthe resulting salts were filtered
3. customThe filtrate was evaporated to an oil which
4. customcrystallized on trituration with pentane
5. filtrationThe solid was filtered
6. customrecrystallized from 1:1 dichloromethane/pentane