反応 #8905

ord-7fd2ced16c8e4fd7949b21830373d6d1

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他then partitioned between EtOAc and water
  2. 2
    洗浄The organic layer was washed with water, brine
  3. 3
    乾燥dried (MgSO4)
  4. 4
    ろ過filtered
  5. 5
    その他evaporated
  6. 6
    その他The residue was purified on a silica gel flash chromatography column
  7. 7
    洗浄eluted with 0–20% EtOAc-hexane
  8. 8
    その他Evaporation of the purified fractions
  9. 9
    その他drying in vacuo

実験手順

A 25 mL rb flask was charged with 1.111 g (2.97 mmol) of the product of Step B, 1.451 g (4.45 mmol) Cs2CO3, 10 mL DMF and finally 0.5 mL (3.71 mmol) of bromopinacolone. The reaction mixture was stirred at room temperature 1 h then partitioned between EtOAc and water. The organic layer was washed with water, brine, then dried (MgSO4), filtered and evaporated. The residue was purified on a silica gel flash chromatography column eluted with 0–20% EtOAc-hexane. Evaporation of the purified fractions and drying in vacuo afforded the title compound.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07091216B2uspto-grants-2006_08