Reaktion #165409

ord-af5d92c52a2140d79ab52bb625bdc812

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturunder reflux
  2. 2
    SonstigeThe organic layer was separated
  3. 3
    Waschenwashed with saturated aqueous sodium chloride
  4. 4
    Trocknendried over anhydrous magnesium sulfate
  5. 5
    Filtrationfiltered
  6. 6
    EinengenThe filtrate was concentrated under a reduced pressure

Vorschrift

A mixture of 4-bromo-2-fluorobenzaldehyde (10 g, 49.3 mmol), ethylene glycol (27.5 mL, 493 mmol), camphorsulfonic acid (115 mg, 0.493 mmol), and toluene (250 mL) was stirred for 5 hours under reflux. The mixture was cooled to room temperature and a saturated sodium hydrogencarbonate aqueous solution was added thereto. The organic layer was separated, washed with saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated under a reduced pressure to obtain the title compound (12.5 g). The title compound was used in the following reaction without any further purification.

Quelle

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