반응 #8302

ord-b0dd637ef9f742f487655199b8f5393a

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The mixture is partitioned between water and ethyl acetate
  2. 2
    기타The layers are separated
  3. 3
    세척the organic layer washed three times with water
  4. 4
    건조once with brine, dried (sodium sulfate)
  5. 5
    여과filtered
  6. 6
    기타evaporated
  7. 7
    기타to give a crude solid
  8. 8
    기타The crude product is recrystallized from ethyl acetate

실험 절차

A solution of 2-methoxy-5-nitrophenol (54.3 g, 321 mmol), benzyl bromide (26.5 mL, 223 mmol,) and cesium carbonate (73 g, 223 mmol) is stirred in N,N-dimethylformamide (250 mL) for 24 h at room temperature. The mixture is partitioned between water and ethyl acetate. The layers are separated and the organic layer washed three times with water, once with brine, dried (sodium sulfate), filtered and evaporated to give a crude solid. The crude product is recrystallized from ethyl acetate to yield the title compound, 56.4 g (68%), as a white crystalline solid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07087626B2uspto-grants-2006_08