Reaktion #2503548

Reaktionsgleichung

2,7-dihydroxy-9-methylfluorene

4-(6-acryloyloxyhexyloxy)benzoic acid

EDC

dichloromethane

→

2,7-bis(4-(6-acryloyloxyhexyl)oxybenzoyloxy)-9-methylfluorene

Ausbeute 10.6%

Lösungsmittel

Water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Waschenthe separated organic layer was washed with water
2. 2
   Trocknendried on anhydrous magnesium sulfate
3. 3
   workup.DISTILLATIONThe solvent was distilled off from this organic layer under reduced pressure
4. 4
   Sonstigethe resulting residue was purified by means of column chromatography (silica gel, eluting solvent: toluene/ethyl acetate [95/5]) and recrystallization (ethanol/ethyl acetate)

Vorschrift

A mixture of 2,7-dihydroxy-9-methylfluorene (0.5 g), 4-(6-acryloyloxyhexyloxy)benzoic acid (1.52 g), EDC (0.99 g), DMAP (5.76 mg) and dichloromethane (30 mL) was stirred at a room temperature for 12 hours. Water was added to the reaction mixture, and the separated organic layer was washed with water and dried on anhydrous magnesium sulfate. The solvent was distilled off from this organic layer under reduced pressure, and the resulting residue was purified by means of column chromatography (silica gel, eluting solvent: toluene/ethyl acetate [95/5]) and recrystallization (ethanol/ethyl acetate) to obtain 2,7-bis(4-(6-acryloyloxyhexyl)oxybenzoyloxy)-9-methylfluorene (0.19 g) of a white solid matter.

Quelle