反応 #41207

反応方程式

4-piperazin-1-yl-phenol

methyl 3-bromo-butyrate

triethylamine

→

title compound

収率 59.3%

3-[4-(4-Hydroxy-phenyl)-piperazin-1-yl]-butyric acid methyl ester

収率 59.3%

溶媒

DMF

反応条件

後処理

1. 1
   workup.ADDITIONThe mixture was poured onto water
2. 2
   抽出extracted with ethyl acetate (50 ml×3)
3. 3
   洗浄The combined organic layers were washed with brine
4. 4
   乾燥dried over anhydrous Na2SO4
5. 5
   その他evaporated under vacuum to dryness
6. 6
   その他The residue was purified by silica gel flash chromatography (1% methanol in CH2Cl2)

実験手順

To a mixture of 4-piperazin-1-yl-phenol (2 g, 11.2 mmol) and methyl 3-bromo-butyrate (2.03 g, 11.2 mmol) in DMF (5 mL) was added triethylamine (4.5 mL, 11.53 mmol) dropwise and the reaction mixture was stirred at ambient temperature overnight. The mixture was poured onto water and extracted with ethyl acetate (50 ml×3). The combined organic layers were washed with brine, dried over anhydrous Na2SO4 and evaporated under vacuum to dryness. The residue was purified by silica gel flash chromatography (1% methanol in CH2Cl2) to furnish the title compound (1.85 g, 59.3%); MS; m/z 279 (M+H).

出典