反应 #41207

ord-8b0039b8c75446b48104676c801868df

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07728032B2uspto-grants-2010_06