反应详情

The general procedure described above was followed when 6'-Hydroxyspiro-(9H-fluorene-9,3'-piperidine)-2'-one (2.7 g) was dissolved in isopropylamine (350 ml) and 10% palladium on charcoal (0.3 g) was added and the vessel pressurized to 90 p.s.i. with hydrogen. The reaction mixture was then heated at 40° for 16 hours and then allowed to cool to room temperature. The catalyst was removed by filtration and the isopropylamine evaporated under reduced pressure. The resulting residue was dissolved in dichloromethane (20 ml) washed with water (2×50 ml), dried with anhydrous sodium sulphate and evaporated to dryness under reduced pressure. The residue was triturated with hexane to give 9-carbamoyl-9-(3-isopropylaminopropyl)fluorene crystals.

1. temperatureThe reaction mixture was then heated at 40° for 16 hours
2. customThe catalyst was removed by filtration
3. customthe isopropylamine evaporated under reduced pressure
4. dissolutionThe resulting residue was dissolved in dichloromethane (20 ml)
5. washwashed with water (2×50 ml)
6. dry with materialdried with anhydrous sodium sulphate
7. customevaporated to dryness under reduced pressure
8. customThe residue was triturated with hexane