반응 #41207

ord-8b0039b8c75446b48104676c801868df

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONThe mixture was poured onto water
  2. 2
    추출extracted with ethyl acetate (50 ml×3)
  3. 3
    세척The combined organic layers were washed with brine
  4. 4
    건조dried over anhydrous Na2SO4
  5. 5
    기타evaporated under vacuum to dryness
  6. 6
    기타The residue was purified by silica gel flash chromatography (1% methanol in CH2Cl2)

실험 절차

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).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07728032B2uspto-grants-2010_06