Reaktion #60031

ord-06cb637d24334ae382e85a7f4772c423

Lösungsmittel

Reaktionsbedingungen

Temperatur
-20°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONTen minutes after addition
  2. 2
    Sonstigethe cooling bath was removed
  3. 3
    workup.ADDITIONWater was carefully added
  4. 4
    Extraktionfollowed by extraction with toluene
  5. 5
    WaschenThe toluene layer was washed with dilute HCl, water, saturated sodium bicarbonate solution
  6. 6
    Sonstigedried
  7. 7
    Einengenconcentrated in vacuo

Vorschrift

A mixture of 2,4-dichlorobenzoyl chloride (4.5 g) and copper (I) iodide (200 mg) in dry THF (30 ml) was cooled to −20° C. under argon. Then a solution of n-propyl magnesium chloride (2 M in ether, 11.0 ml) was added dropwise. Ten minutes after addition was complete, the cooling bath was removed and the mixture stirred for 1 hour. Water was carefully added, followed by extraction with toluene. The toluene layer was washed with dilute HCl, water, saturated sodium bicarbonate solution, dried and concentrated in vacuo to give 1-(2,4-dichlorophenyl)butan-1-one (4.0 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07425557B2uspto-grants-2008_09