反应详情

A solution of 9.0 g (0.019 mole) 2,7-bis(4-piperidinobutyryl)fluorene, 7.54 g (0.0253 mole) sodium dichromate and 300 ml of glacial acetic acid is stirred and refluxed for one hour. The reaction mixture is evaporated to semi-dryness and made basic using concentrated ammonium hydroxide. The solid which precipitates is filtered, washed with water and chromatographed on alumina using chloroform as the eluant. The solvent is removed from the fraction collected, leaving a solid residue which is recrystallized three times from chloroform-acetone to yield 2,7-bis(4-piperidinobutyryl)fluoren-9-one, M.P. 168°-170° C.

1. temperaturerefluxed for one hour
2. customThe reaction mixture is evaporated to semi-dryness
3. customThe solid which precipitates
4. filtrationis filtered
5. washwashed with water
6. customchromatographed on alumina
7. customThe solvent is removed from the fraction
8. customcollected
9. customleaving a solid residue which
10. customis recrystallized three times from chloroform-acetone