Reaktion #1334606

ord-507d461dad264b2bb1db601abe444d01

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe reaction mixture was heated
  2. 2
    Temperaturto reflux during 5 hrs (Dean-Stark trap)
  3. 3
    Temperaturit was cooled
  4. 4
    workup.ADDITIONpoured onto ice
  5. 5
    SonstigeThe organic layer was separated off
  6. 6
    Waschenwashed with 10% KHCO3-solution and brine
  7. 7
    Trocknendried over MgSO4
  8. 8
    Filtrationfiltered
  9. 9
    Einengenconcentrated

Vorschrift

A stirred solution of 2,4-difluorobenzaldehyde (15.4 ml) in toluene (200 ml) was treated with ethylene glycol (23.2 ml) and p-toluene sulfonic acid (0.53 g). The reaction mixture was heated to reflux during 5 hrs (Dean-Stark trap), then it was cooled to r.t and poured onto ice. The organic layer was separated off, washed with 10% KHCO3-solution and brine, dried over MgSO4, filtered and concentrated to give 2-(2,4-difluoro-phenyl)-[1,3]dioxolane (26.8 g) as a light yellow oil. MS 186.1 ([M]+)

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07129238B2uspto-grants-2006_10