反応 #66122

反応方程式

1-(4-nitro-phenyl)-piperazine

pivaloyl chloride

triethylamine

→

2,2-dimethyl-1-[4-(4-nitro-phenyl)-piperazin-1-yl]-propan-1-one

収率 85.8%

溶媒

DCM

DCM

反応条件

後処理

1. 1
   洗浄washed with water (2×50 mL) and brine (50 mL)
2. 2
   乾燥dried over sodium sulfate
3. 3
   濃縮concentrated to dryness

実験手順

To an ice-cooled solution of 1-(4-nitro-phenyl)-piperazine (prepared as described in Reference Example 29; 5 g, 24 mmol) in DCM (40 mL) was added pivaloyl chloride (4.36 g, 36.2 mmol) and triethylamine (8.73 mL, 60 mmol) at 0-5° C. The mixture was warmed to room temperature and stirred for 1 hour then diluted with DCM (150 mL), washed with water (2×50 mL) and brine (50 mL), dried over sodium sulfate and concentrated to dryness to afford 2,2-dimethyl-1-[4-(4-nitro-phenyl)-piperazin-1-yl]-propan-1-one (6 g, 85.7%) as a yellow solid.

出典