反応 #1121732

反応方程式

ethyl 4-bromobutanoate

1-methylpiperazine

K2CO3

→

ethyl 4-(4-methylpiperzin-1-yl)butanoate

収率 96.0%

溶媒

acetonitrile

反応条件

後処理

1. 1
   温度was refluxed for 18 h
2. 2
   濃縮before concentrated in vacuo
3. 3
   その他The organic layer was then separated
4. 4
   抽出the aqueous layer was extracted with dichloromethane (DCM, 3×150 mL)
5. 5
   洗浄The combined organic extracts were washed with water (150 mL)
6. 6
   乾燥dried (Na2SO4)
7. 7
   濃縮concentrated in vacuo

実験手順

A mixture of ethyl 4-bromobutanoate (5.75 g, 29.5 mmol; Aldrich No. 167118) and 1-methylpiperazine (3.55 mL, 32.0 mmol; Aldrich No. 130001) and anhydrous K2CO3 (4.5 g, 32.5 mmol; Fisher No. P208) in acetonitrile (MeCN, 150 mL) was refluxed for 18 h before concentrated in vacuo. The organic layer was then separated and the aqueous layer was extracted with dichloromethane (DCM, 3×150 mL). The combined organic extracts were washed with water (150 mL), dried (Na2SO4), and concentrated in vacuo to give ethyl 4-(4-methylpiperzin-1-yl)butanoate (6.01 g, 96%) as a yellow oil.

出典