Reaktion #2503539

Reaktionsgleichung

Water

2-Pentyloxy-7-(2-(3-fluoro-4-hydroxyphenyl)ethyl)fluorene

acrylic acid

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

→

2-pentyloxy-7-(2-(3-fluoro-4-acryloyloxyphenyl)ethyl)fluorene

Ausbeute 17.6%

Lösungsmittel

chloroform

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeto come back to a room temperature
2. 2
   Sonstigeto separate the solution
3. 3
   Trocknenthe chloroform layer was dried on anhydrous magnesium sulfate
4. 4
   SonstigeA residue obtained
5. 5
   workup.DISTILLATIONby distilling chloroform
6. 6
   Sonstigeoff was purified by means of column chromatography (silica gel, eluting solvent: toluene), and it
7. 7
   Sonstigewas further recrystallized

Vorschrift

2-Pentyloxy-7-(2-(3-fluoro-4-hydroxyphenyl)ethyl)fluorene (0.7 g) and acrylic acid (0.14 g) were dissolved in chloroform (30 mL) and cooled down to 0° C. 1-Ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (0.44 g) and 4-dimethylaminopyridine (0.01 g) were added thereto, and then the temperature was allowed to come back to a room temperature, followed by stirring for 24 hours. Water was added to separate the solution, and the chloroform layer was dried on anhydrous magnesium sulfate. A residue obtained by distilling chloroform off was purified by means of column chromatography (silica gel, eluting solvent: toluene), and it was further recrystallized to obtain 2-pentyloxy-7-(2-(3-fluoro-4-acryloyloxyphenyl)ethyl)fluorene (0.14 g) of the intended product.

Quelle