Реакция #2186193

Уравнение реакции

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

DMF

POCl3

→

desired product

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

Условия реакции

Обработка

1. 1
   Другоеto reach room temperature
2. 2
   Температураheated
3. 3
   workup.STIRRINGstirred for 3 h at 90° C
4. 4
   ДругоеThe reaction mixture is evaporated
5. 5
   Экстракцияthe residue extracted with water and ethyl acetate
6. 6
   ПромывкаThe organic phases are washed with brine
7. 7
   Сушкаdried over sodium sulphate
8. 8
   Другоеevaporated
9. 9
   Другоеchromatographed (silica gel, ethyl acetate followed by ethyl acetate/MeOH 85:15)

Методика

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.

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