반응 #11731

반응 방정식

2-chloro-1-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-ethanone

5-chlorosalicylaldehyde

potassium carbonate

potassium iodide

→

title compound

수율 84.5%

5-Chloro-2-{2-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-2-oxo-ethoxy}-benzaldehyde

수율 84.5%

용매

brine

dimethylformamide

반응 조건

후처리

1. 1
   온도The reaction was cooled
2. 2
   추출extracted with ethyl acetate
3. 3
   건조The organic layer was dried over magnesium sulfate
4. 4
   여과filtered
5. 5
   농축The filtrate was concentrated in vacuo
6. 6
   기타to give crude product
7. 7
   기타Purification via chromatography on silica gel

실험 절차

To a solution of 2-chloro-1-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-ethanone (2.87 g, 9.6 mmol) in dimethylformamide (20 mL) was added 5-chlorosalicylaldehyde (1.65 g, 10.5 mmol), potassium carbonate (2.64 g, 19.2 mmol) and potassium iodide (1.59 g, 9.6 mmol). The resulting mixture was heated to 100° C. for 12 hours. The reaction was cooled, diluted with saturated aqueous brine and extracted with ethyl acetate. The organic layer was dried over magnesium sulfate and filtered. The filtrate was concentrated in vacuo to give crude product. Purification via chromatography on silica gel gave the title compound (3.40 g).

출처