반응 #2186193

반응 방정식

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

DMF

POCl3

→

desired product

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

반응 조건

후처리

1. 1
   기타to reach room temperature
2. 2
   온도heated
3. 3
   workup.STIRRINGstirred for 3 h at 90° C
4. 4
   기타The reaction mixture is evaporated
5. 5
   추출the residue extracted with water and ethyl acetate
6. 6
   세척The organic phases are washed with brine
7. 7
   건조dried over sodium sulphate
8. 8
   기타evaporated
9. 9
   기타chromatographed (silica gel, ethyl acetate followed by ethyl acetate/MeOH 85:15)

실험 절차

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.

출처