反応 #11735

反応方程式

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

potassium iodide

2-(5-chloro-2-hydroxy-benzyl)-isoindole-1,3-dione

potassium carbonate

→

title compound

収率 63.3%

2-(5-Chloro-2-{2-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-2-oxo-ethoxy}-benzyl)-isoindole-1,3-dione

収率 63.3%

溶媒

water

dimethylformamide

反応条件

後処理

1. 1
   温度The reaction was cooled to ambient temperature
2. 2
   抽出extracted with 1:1 diethyl ether/hexanes (3×)
3. 3
   洗浄washed with water and brine
4. 4
   乾燥dried over magnesium sulfate
5. 5
   ろ過filtered
6. 6
   その他evaporated

実験手順

To a solution of 2-chloro-1-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-ethanone (0.75 g, 2.50 mmol) in dry dimethylformamide (25 mL) was added potassium iodide (0.40 g, 2.39 mmol), 2-(5-chloro-2-hydroxy-benzyl)-isoindole-1,3-dione (0.80 g, 2.76 mmol) and potassium carbonate (0.70 g, 5.10 mmol). The resulting mixture was heated to 70° C. for 23 hours. The reaction was cooled to ambient temperature, diluted with water and extracted with 1:1 diethyl ether/hexanes (3×). The organic layers were combined, washed with water and brine, dried over magnesium sulfate, filtered and evaporated to give the title compound (0.87 g).

出典