反応 #165042

ord-10d7af2143ca4d3ca6c724172e57e2f3

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度under reflux for 2 hours and 10 minutes
  2. 2
    濃縮concentrated under a reduced pressure
  3. 3
    その他The residue was purified by silica gel column chromatography (heptane: acetic acid=8:1)

実験手順

A mixture of (4-(pyridin-2-yloxymethyl)-phenyl)methanol (540 mg, 2.51 mmol) described in Manufacturing Example 2-1-1, triphenylphosphine (856 mg, 3.27 mmol) and carbon tetrachloride (10.8 g, 10.2 mmol) was stirred under reflux for 2 hours and 10 minutes. The reaction solution was cooled to room temperature, and concentrated under a reduced pressure. The residue was purified by silica gel column chromatography (heptane: acetic acid=8:1) to obtain the title compound (300 mg, 51.1%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08841327B2uspto-grants-2014_09