Reaktion #1102081

Reaktionsgleichung

sulfuric acid

4-hydroxybenzoic acid

2,7-dihydroxy-9-methylfluorene

boric acid

→

2,7-bis(4-hydroxybenzoyloxy)-9-methylfluorene

Ausbeute 70.0%

Lösungsmittel

xylene

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe mixture was heated
2. 2
   Temperaturunder reflux for 6 hours
3. 3
   Sonstigewhile removing water
4. 4
   FiltrationA solid matter thus deposited was collected by filtration under reduced pressure
5. 5
   Waschenrinsed with toluene
6. 6
   SonstigeThe solid matter was recrystallized from a mixed solvent of ethanol (75 mL) and acetone (75 mL)

Vorschrift

In a nitrogen atmosphere, concentrated sulfuric acid (0.2 mL) was added to a mixture of 4-hydroxybenzoic acid (13.0 g), 2,7-dihydroxy-9-methylfluorene (10.0 g), boric acid (0.3 g) and xylene (120 mL), and the mixture was heated under reflux for 6 hours while removing water. A solid matter thus deposited was collected by filtration under reduced pressure, and rinsed with toluene. The solid matter was recrystallized from a mixed solvent of ethanol (75 mL) and acetone (75 mL) to provide 2,7-bis(4-hydroxybenzoyloxy)-9-methylfluorene (compound [H1]) (14.9 g) in the form of pale rose crystals.

Quelle