反応 #1102081

反応方程式

sulfuric acid

4-hydroxybenzoic acid

2,7-dihydroxy-9-methylfluorene

boric acid

→

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

収率 70.0%

溶媒

xylene

反応条件

後処理

1. 1
   温度the mixture was heated
2. 2
   温度under reflux for 6 hours
3. 3
   その他while removing water
4. 4
   ろ過A solid matter thus deposited was collected by filtration under reduced pressure
5. 5
   洗浄rinsed with toluene
6. 6
   その他The solid matter was recrystallized from a mixed solvent of ethanol (75 mL) and acetone (75 mL)

実験手順

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.

出典