반응 #217453

반응 방정식

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

수율 22.0%

용매

methylene chloride

Water

반응 조건

후처리

1. 1
   건조the resulting organic layer was dried on anhydrous magnesium sulfate
2. 2
   기타A residue obtained
3. 3
   workup.DISTILLATIONby distilling the solvent

실험 절차

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).

출처