تفاعل #2186193

معادلة التفاعل

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

DMF

POCl3

→

desired product

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

ظروف التفاعل

المعالجة

1. 1
   أخرىto reach room temperature
2. 2
   درجة الحرارةheated
3. 3
   workup.STIRRINGstirred for 3 h at 90° C
4. 4
   أخرىThe reaction mixture is evaporated
5. 5
   استخلاصthe residue extracted with water and ethyl acetate
6. 6
   غسيلThe organic phases are washed with brine
7. 7
   تجفيفdried over sodium sulphate
8. 8
   أخرىevaporated
9. 9
   أخرىchromatographed (silica gel, ethyl acetate followed by ethyl acetate/MeOH 85:15)

الإجراء التجريبي

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.

المصدر