Реакция #9548

ord-aae0dad34e834b03a63c256ec63dadca

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеthe vessel was purged with nitrogen
  2. 2
    Другоеfor two hours
  3. 3
    ФильтрацияThe reaction mixture was filtered through a layer of CELITE
  4. 4
    Фильтрацияfilter aid
  5. 5
    Промывкаthe filter cake was washed with acetonitrile
  6. 6
    КонцентрированиеThe filtrate was concentrated under reduced pressure

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07091214B2uspto-grants-2006_08