반응 #9548

ord-aae0dad34e834b03a63c256ec63dadca

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타the vessel was purged with nitrogen
  2. 2
    기타for two hours
  3. 3
    여과The reaction mixture was filtered through a layer of CELITE
  4. 4
    여과filter aid
  5. 5
    세척the filter cake was washed with acetonitrile
  6. 6
    농축The filtrate was concentrated under reduced pressure

실험 절차

A solution of (7-bromo-3-nitroquinolin-4-yl)-(2-methylpropyl)amine (30.9 g, 105 mmol) in acetonitrile (1.8 L) and isopropanol (200 mL) was added to a Parr vessel. A mixture of 5% platinum on carbon (3.0 g) and acetonitrile:isopropanol (20 mL) was added, and the vessel was purged with nitrogen. The vessel was placed under hydrogen pressure (40 psi, 2.8×105 Pa) for two hours. After one hour, the pressure had decreased to 20 psi (1.4×105 Pa) and was readjusted to 40 psi (2.8×105 Pa). The reaction mixture was filtered through a layer of CELITE filter aid, and the filter cake was washed with acetonitrile. The filtrate was concentrated under reduced pressure to provide 7-bromo-N4-(2-methylpropyl)quinoline-3,4-diamine as an oil.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07091214B2uspto-grants-2006_08