Reaktion #10463

Reaktionsgleichung

9-hydroxy-9-fluorenecarboxylic acid

sulphuric acid

sodium hydrogen carbonate

→

methyl 9-hydroxy-fluorene-9-carboxylate

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturrefluxed for 1 hour
2. 2
   workup.ADDITIONare added
3. 3
   workup.DISTILLATIONthe methanol is largely distilled off under reduced pressure
4. 4
   ExtraktionThe residue remaining is extracted with dichloromethane and water
5. 5
   Sonstigethe organic phase is dried
6. 6
   Sonstigeevaporated to dryness

Vorschrift

50.4 g (0.223 mol) 9-hydroxy-9-fluorenecarboxylic acid are dissolved in 500 ml of methanol, combined with 5 ml (0.089 mol) conc. sulphuric acid and refluxed for 1 hour. After cooling 100 ml sodium hydrogen carbonate solution (about pH 8) are added, and the methanol is largely distilled off under reduced pressure. The residue remaining is extracted with dichloromethane and water, the organic phase is dried and evaporated to dryness.

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