反応 #2186193

反応方程式

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

DMF

POCl3

→

desired product

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

反応条件

後処理

1. 1
   その他to reach room temperature
2. 2
   温度heated
3. 3
   workup.STIRRINGstirred for 3 h at 90° C
4. 4
   その他The reaction mixture is evaporated
5. 5
   抽出the residue extracted with water and ethyl acetate
6. 6
   洗浄The organic phases are washed with brine
7. 7
   乾燥dried over sodium sulphate
8. 8
   その他evaporated
9. 9
   その他chromatographed (silica gel, ethyl acetate followed by ethyl acetate/MeOH 85:15)

実験手順

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.

出典