Reaktion #73775

ord-071d2dbb8fcc4578991be19624694c5e

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigequenched by addition of ice
  2. 2
    workup.ADDITIONmethyl t-butyl ether added
  3. 3
    workup.STIRRINGAfter stirring for 1 hour the precipitate
  4. 4
    Filtrationwas collected by filtration
  5. 5
    Waschenwashed with water, methyl t-butyl ether and water

Vorschrift

A suspension of 4-(4-Bromo-phenyl)-piperidin-4-ol (4.02 g, 15.7 mmol) in chlorobenzene (30 ml) was added dropwise to a suspension of aluminium chloride (7.32 g, 54.9 mmol) in chlorobenzene (10 ml) at 0° C. The reaction mixture was stirred at 0° C. for 2 hours, quenched by addition of ice then methyl t-butyl ether added. After stirring for 1 hour the precipitate was collected by filtration washed with water, methyl t-butyl ether and water to afford the title compound (5.59 g, 92% yield). LC/MS: (PS-B3) Rt 3.57 [M+H]+ 350, 352.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08541461B2uspto-grants-2013_09