Reaktion #2298754

Reaktionsgleichung

Water

4-(4-Allyloxybutyloxy)benzoic acid

2,7-dihydroxy-9-methylfluorene

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

→

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

Lösungsmittel

methylene chloride

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeto separate the solution
2. 2
   Trocknenthe organic layer was dried on anhydrous magnesium sulfate
3. 3
   SonstigeA residue obtained
4. 4
   workup.DISTILLATIONafter distilling the solvent
5. 5
   Sonstigerecrystallized from a mixed solvent of ethanol and ethyl acetate

Vorschrift

4-(4-Allyloxybutyloxy)benzoic acid 1.34 g and 2,7-dihydroxy-9-methylfluorene 0.46 g were dissolved in 30 ml of methylene chloride and cooled down to 5° C., and 0.01 g of dimethylaminopyridine and 1.15 g of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride were added thereto, followed by stirring the solution at a room temperature for 12 hours. Water 50 ml was added to separate the solution, and the organic layer was dried on anhydrous magnesium sulfate. A residue obtained after distilling the solvent off was refined by means of silica gel chromatography and recrystallized from a mixed solvent of ethanol and ethyl acetate to obtain 0.6 g of 2,7-di[4-(4-allyloxybutyloxy)benzoyloxy]-9-methylfluorene. Phase transition temperature: C 107 N 222 I

Quelle