Reaktion #70089

Reaktionsgleichung

Potash

5a

[9,9-Dibutyl-7-[2-[4-(dihexylamino)phenyl]ethynyl]-9H-fluorene-2-yl]-2-methyl-3-butyn-2-ol

→

5b

Ausbeute 87.0%

4-[2-(9,9-Dibutyl-7-ethynyl-9H-fluoren-2-yl)ethynyl]-N,N-dihexylbenzenamine

Ausbeute 87.0%

Lösungsmittel

toluene i-PrOH

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe mixture is heated in a reverse-flow boiler for 1 h
2. 2
   TemperaturAfter cooling
3. 3
   Filtrationthe potash is filtered
4. 4
   Sonstigethe solvents are evaporated
5. 5
   SonstigeThe raw product is purified by silica gel column chromatography (heptane/CH2Cl2 90:10)

Vorschrift

Potash powder (0.07 g) is added to a solution of 5a (0.798 g, 1.24 mmol) in 8.75 mL of toluene/i-PrOH (6/1). The mixture is heated in a reverse-flow boiler for 1 h. After cooling, the potash is filtered and the solvents are evaporated. The raw product is purified by silica gel column chromatography (heptane/CH2Cl2 90:10) to yield 0.632 g (87%) of 5b.

Quelle