반응 #1447123

ord-cb8e894fb6f642e68ae41001b4f15a85

반응 조건

온도
210°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    세척The organic phase is again washed with water
  2. 2
    건조dried over magnesium sulphate
  3. 3
    농축concentrated under reduced pressure
  4. 4
    기타Purification by column chromatography (cyclohexane/ethyl acetate 3:1)

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07879760B2uspto-grants-2011_02