Reaktion #684970

ord-278bfaeef23848fbaf87b85f11597d2f

Reaktionsgleichung

O=C([O-])[O-].[K+].[K+]
Potassium carbonate
CI
methyl iodide
CCCC(=O)c1ccc(Br)cc1O
compound
CCCC(=O)c1ccc(Br)cc1O
1-(4-Bromo-2-hydroxyphenyl)-1-butanone
CCCC(=O)c1ccc(Br)cc1OC
title compound
Ausbeute 67.7%
CCCC(=O)c1ccc(Br)cc1OC
1-(4-Bromo-2-methoxyphenyl)-1-butanone
Ausbeute 67.7%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwhile heating
  2. 2
    Temperaturunder reflux for 4 hours
  3. 3
    FiltrationThe reaction mixture was filtered through celite, ether
  4. 4
    workup.ADDITIONwas added
  5. 5
    Sonstigeto remove insoluble material
  6. 6
    Filtrationby filtration
  7. 7
    Einengenthe filtrate was concentrated under reduced pressure
  8. 8
    SonstigeThe residue was purified by silica gel column chromatography

Vorschrift

Potassium carbonate (9.07 g) and methyl iodide (3.92 ml) were added to a solution of the compound of Example B220 (13.30 g) in acetone (75 ml), and this reaction mixture was stirred while heating under reflux for 4 hours. The reaction mixture was filtered through celite, ether was added to remove insoluble material by filtration, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography to give the title compound (9.52 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07897387B2uspto-grants-2011_03