Reaktion #1447123

ord-cb8e894fb6f642e68ae41001b4f15a85

Reaktionsbedingungen

Temperatur
210°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    WaschenThe organic phase is again washed with water
  2. 2
    Trocknendried over magnesium sulphate
  3. 3
    Einengenconcentrated under reduced pressure
  4. 4
    SonstigePurification by column chromatography (cyclohexane/ethyl acetate 3:1)

Vorschrift

A solution comprising 8.0 g (0.045 mol) of 1-(2-aminophenyl)-3-methylbutan-1-one (X-1), 6.8 g (0.135 mol) of hydrazine hydrate and 7.6 g (0.135 mol) of potassium hydroxide in 90 ml of triethylene glycol is heated at 210° C. for 6 h. For work-up, water and ethyl acetate are added at room temperature. The organic phase is again washed with water, dried over magnesium sulphate and concentrated under reduced pressure. Purification by column chromatography (cyclohexane/ethyl acetate 3:1) gives 5.3 g (71.5% of theory) of [2-(3-methylbutyl)-phenyl]amine.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07879760B2uspto-grants-2011_02