Reaktion #52844

ord-121fda83a02d475a9abaa17eaf5c6112

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionextracted with Et2O (3×40 ml)
  2. 2
    WaschenThe combined organic layers were washed with water, sat. aqueous NaHCO3 and brine
  3. 3
    Trocknendried over MgSO4
  4. 4
    Einengenconcentrated in vacuo
  5. 5
    SonstigePurification
  6. 6
    workup.DISTILLATIONby Kugelrohr distillation

Vorschrift

15.0 g (58.3 mmol) of 5-(3-bromophenyl)-2-methylpentan-2-ol (Compound E) was cooled to 0° C. and then 2.8 ml of conc. H2SO4 was added. The mixture was stirred for 2.5 hours, diluted with water (20 ml) and extracted with Et2O (3×40 ml). The combined organic layers were washed with water, sat. aqueous NaHCO3 and brine, dried over MgSO4 and concentrated in vacuo. Purification by Kugelrohr distillation gave the title compound as a colorless oil.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06855832B2uspto-grants-2005_02