Reaktion #2186193

Reaktionsgleichung

3-[4-(2-Fluoro-ethyl)-piperazin-1-yl]-phenol

DMF

POCl3

→

desired product

4-[4-(2-Fluoro-ethyl)piperazin-1 -yl]-2-hydroxy-benzaldehyde

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeto reach room temperature
2. 2
   Temperaturheated
3. 3
   workup.STIRRINGstirred for 3 h at 90° C
4. 4
   SonstigeThe reaction mixture is evaporated
5. 5
   Extraktionthe residue extracted with water and ethyl acetate
6. 6
   WaschenThe organic phases are washed with brine
7. 7
   Trocknendried over sodium sulphate
8. 8
   Sonstigeevaporated
9. 9
   Sonstigechromatographed (silica gel, ethyl acetate followed by ethyl acetate/MeOH 85:15)

Vorschrift

600 mg (2.675 mmol) 3-[4-(2-Fluoro-ethyl)-piperazin-1-yl]-phenol are dissolved in 8 mL DMF and cooled to 0° C. 0.27 mL (1.1 eq) POCl3 is added dropwise within 2 min. and the reaction mixture stirred for an additional 5 min. before being allowed to reach room temperature, and then heated and stirred for 3 h at 90° C. The reaction mixture is evaporated and the residue extracted with water and ethyl acetate. The organic phases are washed with brine, dried over sodium sulphate and evaporated. The residue is column chromatographed (silica gel, ethyl acetate followed by ethyl acetate/MeOH 85:15) to yield the desired product as a yellowish oil.

Quelle