Reaktion #2503547

Reaktionsgleichung

2,7-diacetyloxy-9-methylfluorene

lithium hydroxide monohydrate

hydrochloric acid

→

2,7-dihydroxy-9-methylfluorene

Ausbeute 84.2%

Lösungsmittel

ethylene glycol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas refluxed for one hour
2. 2
   Temperaturby heating
3. 3
   Extraktionextracted with ethyl acetate
4. 4
   WaschenThe organic layer was sufficiently washed with water
5. 5
   Trocknendried on anhydrous magnesium sulfate
6. 6
   workup.DISTILLATIONThe solvent was distilled off from this organic layer under reduced pressure

Vorschrift

A mixture of 2,7-diacetyloxy-9-methylfluorene (12 g), lithium hydroxide monohydrate (3.42 g) and ethylene glycol (120 mL) was refluxed for one hour by heating. The reaction mixture was poured into 6M-hydrochloric acid and extracted with ethyl acetate. The organic layer was sufficiently washed with water and then dried on anhydrous magnesium sulfate. The solvent was distilled off from this organic layer under reduced pressure to obtain 2,7-dihydroxy-9-methylfluorene (7.24 g) of light brown crystal. Melting point: 191.5-196.3° C.

Quelle