反応 #11731

反応方程式

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

5-chlorosalicylaldehyde

potassium carbonate

potassium iodide

→

title compound

収率 84.5%

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

収率 84.5%

溶媒

brine

dimethylformamide

反応条件

後処理

1. 1
   温度The reaction was cooled
2. 2
   抽出extracted with ethyl acetate
3. 3
   乾燥The organic layer was dried over magnesium sulfate
4. 4
   ろ過filtered
5. 5
   濃縮The filtrate was concentrated in vacuo
6. 6
   その他to give crude product
7. 7
   その他Purification via chromatography on silica gel

実験手順

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).

出典