反应详情

0.34 Gram of aluminum lithium hydride was suspended in 30 ml of THF and to the suspension was gradually added dropwise 1.6 g of 8-hydroxy-5,7-dimethyl 9-(2-oxo-1-pyrrolidinyl)-1,2,3,4,4a,9a-hexahydrofluorene. This suspension was refluxed with heating for 5 hours and then ice-cooled and excess hydride was decomposed with ethyl acetate. To the reaction mixture was added 1.5 ml of saturated aqueous sodium sulfate solution, followed by stirring at room temperature for 1 hour and then filtration to remove the precipitate. The filtrate was concentrated and to the residue was added ethyl acetate and insoluble matter was removed by filtration. The filtrate was again concentrated and the residue was recrystallized from hydrous ethanol to obtain 1.06 g of 8-hydroxy-5,7-dimethyl-9-(1-pyrrolidinyl)-1,2,3,4,4a,9a-hexahydrofluorene having a melting point of 96°-97° C. and of colorless prism-like crystal.

1. temperatureThis suspension was refluxed
2. temperaturewith heating for 5 hours
3. temperatureice-cooled
4. filtrationfiltration
5. customto remove the precipitate
6. concentrationThe filtrate was concentrated and to the residue
7. additionwas added ethyl acetate and insoluble matter
8. customwas removed by filtration
9. concentrationThe filtrate was again concentrated
10. customthe residue was recrystallized from hydrous ethanol