反応 #11728

反応方程式

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

2-nitro-4-chlorophenol

potassium carbonate

potassium iodide

→

title compound

収率 92.5%

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

収率 92.5%

溶媒

water

butanone

反応条件

後処理

1. 1
   温度The reaction mixture was heated
2. 2
   温度at reflux overnight
3. 3
   温度The reaction mixture was then cooled
4. 4
   抽出extracted with ethyl acetate
5. 5
   乾燥The organic layer was dried over magnesium sulfate
6. 6
   ろ過filtered
7. 7
   濃縮concentrated
8. 8
   その他to give an orange oil

実験手順

To a solution of 2-chloro-1-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-ethanone (1.0 g, 3.35 mmol) in butanone (35 mL) was added 2-nitro-4-chlorophenol (0.64 g, 3.69 mmol), potassium carbonate (0.93 g, 6.7mmol) and potassium iodide (0.56 g, 3.35 mmol). The reaction mixture was heated at reflux overnight. The reaction mixture was then cooled, diluted with water and extracted with ethyl acetate. The organic layer was dried over magnesium sulfate, filtered and concentrated to give an orange oil. Chromatography on silica gel gave the title compound (1.35 g).

出典