反応 #2503548

反応方程式

2,7-dihydroxy-9-methylfluorene

4-(6-acryloyloxyhexyloxy)benzoic acid

EDC

dichloromethane

→

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

収率 10.6%

溶媒

Water

反応条件

後処理

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

実験手順

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.

出典