反応 #217453

反応方程式

Dimethylaminopyridine

1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride

4-(4-allyloxybutyloxy)benzoic acid

2-(4-octyloxybenzoyloxy)-7-hydroxy-9-methylfluorene

→

2-[4-(4-allyloxybutyloxy)benzoyloxy]-7-(4-octyloxybenzoyloxy)-9-methylfluorene

収率 22.0%

溶媒

methylene chloride

Water

反応条件

後処理

1. 1
   乾燥the resulting organic layer was dried on anhydrous magnesium sulfate
2. 2
   その他A residue obtained
3. 3
   workup.DISTILLATIONby distilling the solvent

実験手順

Dimethylaminopyridine 0.01 g and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride 0.8 g were added to a methylene chloride (50 ml) solution of 4-(4-allyloxybutyloxy)benzoic acid 0.84 g and 2-(4-octyloxybenzoyloxy)-7-hydroxy-9-methylfluorene (J1) 1.5 g while maintaining 5° C., and the mixture was further stirred at room temperature for 12 hours. Water 50 ml was added thereto, and the resulting organic layer was dried on anhydrous magnesium sulfate. A residue obtained by distilling the solvent off was refined by silica gel column chromatography to obtain 0.5 g of 2-[4-(4-allyloxybutyloxy)benzoyloxy]-7-(4-octyloxybenzoyloxy)-9-methylfluorene (J2).

出典