Reaktion #165052

ord-851bb41524274c81898e186bee7adc52

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturunder reflux for 7 hours
  2. 2
    Einengenconcentrated under a reduced pressure
  3. 3
    SonstigeThe residue was purified by neutral silica gel column chromatography (ethyl acetate:heptane=1:15)

Vorschrift

A mixture of (4-butoxymethyl-phenyl)-methanol (190 mg, 0.98 mmol) described in Manufacturing Example 33-1-3, triphenylphosphine (310 mg, 1.2 mmol) and carbon tetrachloride (3 mL) was stirred under reflux for 7 hours. The reaction mixture was cooled to room temperature, and concentrated under a reduced pressure. The residue was purified by neutral silica gel column chromatography (ethyl acetate:heptane=1:15) to obtain the title compound (180 mg, 86%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08841327B2uspto-grants-2014_09