Reaktion #326816

ord-ace5b2838ae24354b374e3cb75638ee3

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONwas added
  2. 2
    Temperaturthe reaction mixture was cooled to 0° C.
  3. 3
    Sonstigequenched with dilute HCl
  4. 4
    Extraktionextracted with ethyl acetate
  5. 5
    TrocknenThe organic layer was dried over sodium sulphate
  6. 6
    Einengenconcentrated under reduced pressure

Vorschrift

To a ice-cold solution of ethyl magnesium iodide prepared from magnesium (2.39 g, 98.51 mmoles) and ethyl iodide (7.88 ml, 98.51 mmoles) in diethyl ether (50 ml), 4-bromo-2-fluorobenzaldehyde(5 g, 24.62 mmoles) in diethyl ether(10 ml) was added and warmed to room temperature. After 12 h, the reaction mixture was cooled to 0° C., quenched with dilute HCl and extracted with ethyl acetate. The organic layer was dried over sodium sulphate and concentrated under reduced pressure to afford the title compound as red colour liquid (5.8 g, 99% yield) which is used as such for step.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08642607B2uspto-grants-2014_02