Reacción #2186193

Ecuación de reacción

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

DMF

POCl3

→

desired product

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

Condiciones de reacción

Tratamiento posterior

1. 1
   Otroto reach room temperature
2. 2
   Temperaturaheated
3. 3
   workup.STIRRINGstirred for 3 h at 90° C
4. 4
   OtroThe reaction mixture is evaporated
5. 5
   Extracciónthe residue extracted with water and ethyl acetate
6. 6
   LavadoThe organic phases are washed with brine
7. 7
   Secadodried over sodium sulphate
8. 8
   Otroevaporated
9. 9
   Otrochromatographed (silica gel, ethyl acetate followed by ethyl acetate/MeOH 85:15)

Procedimiento

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.

Fuente